WO2014103939A1 - Barreau de silicium polycristallin et son procédé de fabrication - Google Patents

Barreau de silicium polycristallin et son procédé de fabrication Download PDF

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Publication number
WO2014103939A1
WO2014103939A1 PCT/JP2013/084275 JP2013084275W WO2014103939A1 WO 2014103939 A1 WO2014103939 A1 WO 2014103939A1 JP 2013084275 W JP2013084275 W JP 2013084275W WO 2014103939 A1 WO2014103939 A1 WO 2014103939A1
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Prior art keywords
core wire
silicon
reactor
silicon core
polycrystalline silicon
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PCT/JP2013/084275
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English (en)
Japanese (ja)
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哲也 井村
恭正 相本
晴之 石田
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株式会社トクヤマ
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Priority to JP2014554415A priority Critical patent/JP6328565B2/ja
Publication of WO2014103939A1 publication Critical patent/WO2014103939A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/02—Silicon
    • C01B33/021—Preparation
    • C01B33/027—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
    • C01B33/035—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition or reduction of gaseous or vaporised silicon compounds in the presence of heated filaments of silicon, carbon or a refractory metal, e.g. tantalum or tungsten, or in the presence of heated silicon rods on which the formed silicon is deposited, a silicon rod being obtained, e.g. Siemens process

Definitions

  • the present invention relates to a polycrystalline silicon rod and a manufacturing method thereof.
  • Various methods for producing silicon used as a raw material for semiconductors or wafers for photovoltaic power generation are known, some of which have already been industrially implemented.
  • One of the methods is a method called a Siemens method, which is connected to the electrode inside a so-called bell jar type reactor comprising a bottom plate and a cover provided with at least a pair of electrodes for energizing the silicon core wire.
  • the arranged silicon core wire is heated to a silicon deposition temperature by energization, and a gas of a silane compound such as trichlorosilane (SiHCl 3 ) or monosilane (SiH 4 ) and hydrogen are supplied thereto, and silicon is deposited by chemical vapor deposition.
  • SiHCl 3 trichlorosilane
  • SiH 4 monosilane
  • a silicon core wire is usually obtained by processing a part of a polycrystalline silicon rod or the like into a thin rod shape. For this reason, an oxide film is generated on the surface of the silicon core wire after the silicon core wire is in contact with the outside air until the process of depositing silicon on the silicon core wire starts. Has been confirmed. For this reason, the polycrystalline silicon rod obtained by the chemical vapor deposition method has a problem that the oxygen concentration at the interface of the silicon core wire is high, and the purity of the silicon as a whole is reduced.
  • Patent Document 1 discloses a method for producing a polycrystalline silicon rod by a chemical vapor deposition method. Under the conditions of high pressure and a large amount of raw material supply, a silicon rod is produced at a high growth rate and yield while preventing fusing of the rod. The purpose is to grow large diameter. However, there is no disclosure about improving the purity of the polycrystalline silicon rod.
  • the present invention provides a polycrystalline silicon rod obtained by vapor-phase growth on a silicon core wire, wherein the oxygen concentration at the silicon core wire interface is reduced, and a method for producing the polycrystalline silicon rod. It is intended to provide.
  • the present inventors have replaced the gas in the reactor with hydrogen before the start of the supply of the silicon deposition source gas, and set the surface temperature of the silicon core wire to a predetermined value. It was found that the oxygen concentration at the interface of the silicon core wire was reduced by maintaining the temperature within the temperature range, and the present invention was completed.
  • the present invention is a polycrystalline silicon rod obtained by vapor phase growth on a silicon core wire, wherein the oxygen concentration at the silicon core wire interface is 5 to 200 ppba.
  • a silicon core wire having both ends connected to the electrode is disposed in a reactor having at least one pair of electrodes, and after the start of preheating in the reactor, A method for producing a polycrystalline silicon rod in which a silicon deposition source gas is supplied into the reactor while energizing a silicon core wire, and polycrystalline silicon is deposited on the silicon core wire, Before the supply of the raw material gas for silicon deposition, the gas in the reactor is replaced with hydrogen, and the surface temperature of the silicon core wire is 900 to 1400 ° C., and the oxide film on the surface of the silicon core wire is removed. It is characterized by holding for a predetermined time.
  • a polycrystalline silicon rod having a reduced oxygen concentration at the silicon core interface can be obtained.
  • the polycrystalline silicon rod according to the present invention preferably has a carbon concentration of 5 to 100 ppba at the silicon core wire interface.
  • the nitrogen concentration at the silicon core interface is 15 ppba or less.
  • the inside of the reactor is preheated by a carbon heater, and after removing the oxide film at the silicon core interface, the gas in the reactor is replaced again with hydrogen.
  • the polycrystalline silicon rod of the present invention has an oxygen concentration of 5 to 200 ppba at the silicon core wire interface. This means that it is suitable for use in semiconductor applications where higher purity and higher quality silicon crystals are required compared to polycrystalline silicon rods of the same weight.
  • FIG. 1 is a schematic cross-sectional view of a polycrystalline silicon rod according to an embodiment of the present invention.
  • FIG. 2 is a schematic view of a polycrystalline silicon rod manufacturing apparatus according to an embodiment of the present invention.
  • FIG. 3 is a graph showing experimental conditions of the example.
  • the polycrystalline silicon rod 20 according to the present embodiment is formed by depositing polycrystalline silicon around the silicon core wire 10 as schematically shown in cross section in FIG.
  • Polycrystalline silicon also called polysilicon, is an aggregate of fine silicon crystals.
  • the diameter of the polycrystalline silicon rod is not particularly limited, but is preferably 75 to 180 mm, more preferably 100 to 160 mm, and still more preferably 110 to 150 mm. As the diameter increases, a larger amount of polycrystalline silicon rods can be obtained in a single manufacturing process.
  • the silicon core wire 10 is manufactured by, for example, separately manufactured polycrystalline silicon, single crystal silicon, or melt-solidified silicon, and is obtained by cutting a rod-shaped member from polycrystalline silicon or the like.
  • the cross-sectional shape in the short direction of the silicon core wire 10 may be any of a circular shape, an elliptical shape, a substantially rectangular shape, or a polygonal shape.
  • the length of one side is preferably about 5 to 15 mm, more preferably 6 to 12 mm, and still more preferably 7 to 10 mm.
  • the length of the diameter is preferably about 5 to 15 mm, more preferably 6 to 12 mm, and still more preferably 7 to 10 mm.
  • the element concentration of oxygen, carbon, nitrogen or the like at the silicon core interface 11 refers to a value obtained by measuring the silicon core interface 11 on the rod cross section by IR (infrared absorption spectrum).
  • the silicon core wire interface refers to a range of 1 mm adjacent to the core wire surface in the deposited layer growing from the core wire surface toward the outer surface of the silicon rod.
  • the oxygen, carbon, and nitrogen concentrations are usually the highest near the silicon core interface and decrease toward the outer surface of the rod, but the IR is measured within the narrow range adjacent to the core surface. In this case, the concentration fluctuation of each element is small and substantially the same value can be obtained.
  • the polycrystalline silicon rod of this embodiment can be obtained by the Siemens method in which the polycrystalline silicon deposition conditions are controlled.
  • a production apparatus having a reactor 2 generally called a bell jar as schematically shown in FIG. 2 is used.
  • the reactor 2 has a bell jar type cover 4 that is detachably connected to the bottom plate 6.
  • at least a pair of electrodes 12 are attached to the bottom plate 6.
  • the number of electrodes 12 is determined according to the number of silicon core wires 10 installed in the reactor 2.
  • the silicon core wire 10 installed inside the reactor 2 is installed in an inverted U shape so as to connect a pair of electrodes 12 to each other, and can be energized via the electrodes 12.
  • the electrode is made of carbon, SUS, Cu or the like.
  • the inverted U-shaped silicon core wire 10 may be formed by connecting a plurality of silicon core wires 10.
  • the rods 20 are formed in a number corresponding to the number of silicon core wires 10.
  • the cover 4 may have a structure in which a ceiling part and a side part are integrated, or may be a structure in which the cover 4 is joined by a flange or welding.
  • the cover 4 is preferably provided with at least one transparent and heat resistant window member 8 through which the inside of the reactor 2 can be observed.
  • a non-contact thermometer 38 such as an infrared temperature sensor may be installed outside the window member 8.
  • the thermometer 38 is capable of measuring the surface temperature of each of the silicon core wire 10 and the rod 20 disposed inside the reactor 2, and the measured temperature signal is a control disposed outside the reactor 2. Input to device 32.
  • a source gas flow rate control (not shown) for adjusting the flow rate of the gas supplied from the source gas supply port 14 into the reactor 2 is shown.
  • the part is attached.
  • a plurality of source gas supply ports 14 and reaction gas discharge ports 16 may be provided in a single reactor 2.
  • the cover 4 and the bottom plate 6 are made of, for example, a heat-resistant member such as stainless steel metal, carbon steel, nickel-based alloy, iron and a composite material of those other metals, a heat-resistant member such as quartz, It has a double structure consisting of an outer surface.
  • a cooling passage is formed inside each of the double structure of the cover 4 and the bottom plate 6, and the cover 4 and the bottom plate 6 supply the refrigerant from the refrigerant supply port 15 and discharge the refrigerant from the refrigerant discharge port 17. They are connected by a connecting part 9.
  • the refrigerant is not particularly limited, and includes a liquid heat medium generally used for cooling, such as water, heat medium oil such as Barrel Therm (trade name: manufactured by Muramatsu Oil Co., Ltd.), and of these, water is particularly preferable. .
  • the inlet refrigerant temperature at the refrigerant supply port 15 is not particularly limited, but is preferably 30 to 200 ° C. when the refrigerant is water.
  • the refrigerant may be circulated under high pressure conditions so that the refrigerant does not vaporize in the cooling passage.
  • a refrigerant flow rate control unit 42 for adjusting the flow rate of the refrigerant supplied from the refrigerant supply port 15 to the inside of the reactor 2 is mounted.
  • the refrigerant flow rate control unit 42 is controlled by the control device 32, and includes, for example, an electromagnetic valve, an air operation valve, a hydraulic operation valve, and an electric valve.
  • a temperature detecting unit 50 for detecting the temperature of the refrigerant supplied from the refrigerant supply port 15 to the inside of the reactor 2 is mounted.
  • the temperature detection part 52 is also attached to the discharge line through which the refrigerant discharged from the refrigerant discharge port 17 passes, and the temperature of the refrigerant discharged from the reactor 2 to the refrigerant discharge port 17 can be detected.
  • the detected temperature signal is input to the control device 32 arranged outside the reactor 2.
  • the refrigerant discharged from the refrigerant discharge port 17 is recooled by a heat exchanger (not shown), adjusted in temperature, and returned to the refrigerant supply port 15.
  • the used refrigerant may be used for other purposes.
  • a power supply means 30 is connected to the electrode 12 connected to the silicon core wire 10.
  • the power supply means is not particularly limited, and is constituted by, for example, a transformer, a battery, a thyristor, an IGBT or the like.
  • the power supply means 30 is controlled by the control device 32.
  • the gas in the reactor 2 is replaced with hydrogen, and the surface temperature of the silicon core wire 10 is maintained at 900 to 1400 ° C.
  • the method for adjusting the surface temperature of the silicon core wire 10 is not particularly limited. Initially, the inside of the reactor is preheated by a carbon heater or a silicon heater, and then energization to the silicon core wire 10 is started via the electrode 12. Then, the silicon core wire 10 is energized and heated.
  • the inside of the reactor 2 is replaced with hydrogen, and the surface temperature of the silicon core wire 10 is maintained at 900 to 1400 ° C., whereby the oxide film on the surface of the silicon core wire 10 is removed.
  • the holding time of the predetermined temperature related to the surface temperature of the silicon core wire may be a time sufficient for removing the oxide film.
  • the time sufficient for removing the oxide film it may be determined empirically by repeating the experiment, or theoretically by thermodynamic calculation.
  • silane gas and a reducing gas are supplied into the reactor 2 from the source gas supply port 14 into the reactor 2 and the reaction of these silicon deposition source gases is performed. Silicon is generated by (reduction reaction of silane).
  • silane gas and reducing gas or “silane gas only” are collectively referred to as “silicon deposition raw material gas”.
  • the silicon deposition temperature is about 600 ° C. or higher
  • the silicon core wire 10 is used while the silicon deposition source gas is supplied into the reactor 2 in order to rapidly deposit silicon on the silicon core wire 10.
  • the silicon core wire 10 is energized and heated so that the surface temperature of the wire becomes about 950 to 1150 ° C.
  • a gas of a silane compound such as monosilane, trichlorosilane, silicon tetrachloride, monochlorosilane, dichlorosilane or the like is used, and in general, trichlorosilane gas is preferably used.
  • hydrogen gas is usually used as the reducing gas. Taking the case of using trichlorosilane gas and hydrogen gas as an example, this reduction reaction is represented by the following formula.
  • a reducing gas (hydrogen gas) is generally used excessively.
  • silicon is also generated by thermal decomposition of trichlorosilane as described below.
  • Silicon (Si) generated by the above reaction is deposited on the silicon core wire 10, and by continuing this reaction, silicon on the silicon core wire 10 grows and finally consists of polycrystalline silicon.
  • the rod 20 will be obtained.
  • the reaction is terminated, the energization to the silicon core wire 10 is stopped, and unreacted silane gas, hydrogen gas, and by-product four are generated from the reactor 2.
  • the bell jar type cover 4 is opened and the rod 20 is taken out.
  • the gas in the reactor 2 is replaced with hydrogen and the surface temperature of the silicon core wire 10 is maintained at 900 to 1400 ° C.
  • the oxide film generated on the surface of the silicon core wire 10 is removed, and in the finally obtained polycrystalline silicon rod, the oxygen concentration at the silicon core wire interface 11 is reduced, and a high-purity polycrystalline silicon rod can be obtained.
  • a polycrystalline silicon rod having an oxygen concentration of 5 to 200 ppba, preferably 5 to 150 ppba at the silicon core interface can be obtained.
  • the surface temperature of the silicon core wire 10 is preferably maintained at 1000 to 1400 ° C., more preferably 1050 to 1400 ° C., before supplying the silicon deposition source gas into the reactor 2.
  • the silicon core wire 10 is placed in the reactor 2 filled with nitrogen, so that nitrogen adheres to the surface of the silicon core wire 10 and the resulting polycrystalline silicon is obtained.
  • the silicon core wire interface 11 of the rod tended to increase the nitrogen concentration in addition to the oxygen concentration.
  • the gas in the reactor 2 is replaced with hydrogen before the silicon deposition source gas is supplied into the reactor 2.
  • the adhesion of nitrogen to the surface of the silicon core wire 10 can be prevented, the nitrogen concentration at the silicon core wire interface 11 of the finally obtained polycrystalline silicon rod can be reduced, and a high-purity polycrystalline silicon rod can be obtained.
  • a polycrystalline silicon rod having a nitrogen concentration at the silicon core wire interface of 15 ppba or less, preferably 10 ppba or less can be obtained.
  • the supply amount of hydrogen that replaces the gas in the reactor 2 before the supply of the silicon deposition source gas is not particularly limited, but the average production amount of polycrystalline silicon rods per reactor is 20 kg / hour or more.
  • the hydrogen supply amount is preferably 0.5 ⁇ hydrogen supply amount [m 3 ] / reactor volume [m 3 ] ⁇ 10, more preferably 2 ⁇ hydrogen supply.
  • the reactor 2 when the reactor 2 is preheated with a carbon heater, methane gas generated by the preheating of the carbon heater adheres to the silicon core wire 10, and the silicon core interface 11 of the resulting polycrystalline silicon rod has oxygen concentration and nitrogen content. In addition to the concentration, the carbon concentration tended to increase.
  • the inside of the reactor 2 is re-substituted with hydrogen.
  • the methane gas generated by the preheating of the carbon heater can be expelled from the reactor 2, and the methane gas, that is, the carbon component on the silicon core wire 10 is prevented from adhering to the silicon core wire interface of the polycrystalline silicon rod finally obtained.
  • the carbon concentration of 11 can be reduced, and a polycrystalline silicon rod with high purity can be obtained.
  • a polycrystalline silicon rod having a carbon concentration at the silicon core wire interface of 5 to 100 ppba, preferably 5 to 50 ppba, more preferably 8 to 35 ppba can be obtained.
  • the supply amount of hydrogen for resubstituting the gas in the reactor 2 is not particularly limited.
  • the production amount of polycrystalline silicon rods per reactor is 20 kg / hour or more on average, it is preferably set to 0. It is preferred that 5 ⁇ hydrogen supply amount [m 3 ] / reactor volume [m 3 ] ⁇ 10, more preferably 2 ⁇ hydrogen supply amount [m 3 ] / reactor volume [ m 3 ] ⁇ 8.
  • Sample 1 An inverted U-shaped silicon core wire 10 having a height of 2000 mm was prepared in a reactor 2 with 10 rods (5 inverted U-shaped pairs) standing up.
  • preheating of the reactor 2 was started with a carbon heater, and then the silicon core wire 10 was electrically heated to maintain the surface temperature of the silicon core wire 10 at a predetermined temperature in the range of 900 to 1400 ° C.
  • the holding time was 1.0 hour sufficient for removing the oxide film on the surface of the silicon core wire 10.
  • the flow rate of the refrigerant flowing through the cooling passage 9 provided in the cover 4 and the bottom plate 6 was appropriately adjusted.
  • the time schedule from preheating to control stop was as shown in FIG. Note that the time-dependent changes in “output of preheating heater”, “output of power supply”, and “surface temperature of rod” shown in FIG.
  • the “change in atmosphere in the reactor” relates to each of the samples 1 to 4, and corresponds to the time schedule described in the upper part of FIG.
  • the obtained polycrystalline silicon rod was cut in the short direction to obtain a cross section of the rod, and the oxygen concentration, carbon concentration and nitrogen concentration at the silicon core interface were measured by IR (infrared absorption spectrum). The results are shown in Table 1.
  • Sample 2 A polycrystalline silicon rod was obtained in the same manner as in Sample 1 except that the surface temperature of the silicon core wire was kept at 800 ° C. after starting the energization heating of the silicon core wire 10 and before supplying the raw material gas for silicon deposition. The oxygen concentration, carbon concentration and nitrogen concentration were measured. The results are shown in Table 1.
  • Sample 3 A polycrystalline silicon rod was obtained and the oxygen concentration, carbon concentration and nitrogen concentration at the silicon core interface were measured in the same manner as Sample 1, except that the hydrogen in the reactor after the removal of the oxide film was not replaced again. . The results are shown in Table 1.
  • Sample 4 A polycrystalline silicon rod was obtained in the same manner as in Sample 1 except that the inside of the reactor before preheating was not replaced with hydrogen, and the oxygen concentration, carbon concentration and nitrogen concentration at the silicon core interface were measured. The results are shown in Table 1.
  • the surface temperature of the silicon core wire is kept at a predetermined temperature within the range of 900 to 1400 ° C. after starting the energization of the silicon core wire 10 from the sample 1 and sample 2 (sample 1), the surface temperature of the silicon core wire is set to 800 ° C. It was confirmed that the oxygen concentration at the silicon core wire interface was lower than that in the case of holding (Sample 2).
  • Sample 5 A polycrystalline silicon rod was obtained in the same manner as Sample 1 except that the surface temperature of the silicon core wire was kept at 1000 ° C. after starting the energization heating of the silicon core wire 10 and before supplying the raw material gas for silicon deposition. The oxygen concentration, carbon concentration and nitrogen concentration were measured. The results are shown in Table 2.
  • Sample 6 A polycrystalline silicon rod was obtained in the same manner as Sample 1 except that the surface temperature of the silicon core wire was kept at 1050 ° C. after the start of energization heating of the silicon core wire 10 and before the supply of the raw material gas for silicon deposition. The oxygen concentration, carbon concentration and nitrogen concentration were measured. The results are shown in Table 2.
  • Sample 7 A polycrystalline silicon rod was obtained in the same manner as Sample 1 except that the surface temperature of the silicon core wire was maintained at 1100 ° C. after the start of energization heating of the silicon core wire 10 and before the supply of the raw material gas for silicon deposition. The oxygen concentration, carbon concentration and nitrogen concentration were measured. The results are shown in Table 2.
  • Sample 8 A polycrystalline silicon rod was obtained in the same manner as Sample 1 except that the surface temperature of the silicon core wire was maintained at 1400 ° C. after the start of energization heating of the silicon core wire 10 and before the supply of the raw material gas for silicon deposition. The oxygen concentration, carbon concentration and nitrogen concentration were measured. The results are shown in Table 2.
  • Sample 9 A polycrystalline silicon rod was obtained and the oxygen concentration, carbon concentration, and nitrogen concentration at the silicon core interface were measured in the same manner as in Sample 7, except that the hydrogen in the reactor after the oxide film removal was not replaced again. .
  • the results are shown in Table 2.
  • Sample 10 A polycrystalline silicon rod was obtained in the same manner as Sample 7 except that the inside of the reactor before preheating was not replaced with hydrogen, and the oxygen concentration, carbon concentration and nitrogen concentration at the silicon core interface were measured. The results are shown in Table 2.
  • Sample 11 Supply of hydrogen at the time of re-replacement of hydrogen in the reactor after the oxide film is removed after the surface temperature of the silicon core wire is maintained at 1100 ° C. after the start of energization heating of the silicon core wire 10 and before supply of the raw material gas for silicon deposition.
  • Sample 12 Supply of hydrogen at the time of re-replacement of hydrogen in the reactor after the oxide film is removed after the surface temperature of the silicon core wire is maintained at 1100 ° C. after the start of energization heating of the silicon core wire 10 and before supply of the raw material gas for silicon deposition.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Silicon Compounds (AREA)

Abstract

L'objet de la présente invention consiste à fournir un barreau de silicium polycristallin qui est obtenu par dépôt en phase vapeur sur un fil de noyau de silicium, et dont la concentration en oxygène au niveau de l'interface du fil de noyau de silicium est réduite. La présente invention concerne un barreau de silicium polycristallin obtenu par dépôt en phase vapeur sur un fil de noyau de silicium, la concentration en oxygène au niveau de l'interface du fil de noyau de silicium étant de 5 à 200 parties atomiques par milliard.
PCT/JP2013/084275 2012-12-27 2013-12-20 Barreau de silicium polycristallin et son procédé de fabrication WO2014103939A1 (fr)

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JP2016121052A (ja) * 2014-12-25 2016-07-07 信越化学工業株式会社 多結晶シリコン棒、多結晶シリコン棒の加工方法、多結晶シリコン棒の結晶評価方法、および、ｆｚ単結晶シリコンの製造方法
WO2017221952A1 (fr) 2016-06-23 2017-12-28 三菱マテリアル株式会社 Tige de silicium polycristallin et son procédé de fabrication
CN113387360A (zh) * 2021-05-25 2021-09-14 河南硅烷科技发展股份有限公司 一种抑制区熔级多晶硅cvd过程中硅枝晶生长的界面浸润性调控方法
US11440803B2 (en) 2016-12-14 2022-09-13 Wacker Chemie Ag Process for preparing polycrystalline silicon
US11667533B2 (en) 2016-12-14 2023-06-06 Wacker Chemie Ag Process for preparing polycrystalline silicon

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Publication number Priority date Publication date Assignee Title
JP2016121052A (ja) * 2014-12-25 2016-07-07 信越化学工業株式会社 多結晶シリコン棒、多結晶シリコン棒の加工方法、多結晶シリコン棒の結晶評価方法、および、ｆｚ単結晶シリコンの製造方法
US10800659B2 (en) 2014-12-25 2020-10-13 Shin-Etsu Chemical Co., Ltd. Polycrystalline silicon rod, processing method for polycrystalline silicon rod, method for evaluating polycrystalline silicon rod, and method for producing FZ single crystal silicon
US11167994B2 (en) 2014-12-25 2021-11-09 Shin-Etsu Chemical Co., Ltd. Polycrystalline silicon rod, processing method for polycrystalline silicon rod, method for evaluating polycrystalline silicon rod, and method for producing FZ single crystal silicon
WO2017221952A1 (fr) 2016-06-23 2017-12-28 三菱マテリアル株式会社 Tige de silicium polycristallin et son procédé de fabrication
KR20190019053A (ko) 2016-06-23 2019-02-26 미쓰비시 마테리알 가부시키가이샤 다결정 실리콘 로드 및 그 제조 방법
US11306001B2 (en) 2016-06-23 2022-04-19 Mitsubishi Materials Corporation Polycrystalline silicon rod and method for producing same
US11440803B2 (en) 2016-12-14 2022-09-13 Wacker Chemie Ag Process for preparing polycrystalline silicon
US11667533B2 (en) 2016-12-14 2023-06-06 Wacker Chemie Ag Process for preparing polycrystalline silicon
CN113387360A (zh) * 2021-05-25 2021-09-14 河南硅烷科技发展股份有限公司 一种抑制区熔级多晶硅cvd过程中硅枝晶生长的界面浸润性调控方法

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