WO2008065829A1 - Dispositif de production de trichlorosilane - Google Patents

Dispositif de production de trichlorosilane Download PDF

Info

Publication number
WO2008065829A1
WO2008065829A1 PCT/JP2007/070446 JP2007070446W WO2008065829A1 WO 2008065829 A1 WO2008065829 A1 WO 2008065829A1 JP 2007070446 W JP2007070446 W JP 2007070446W WO 2008065829 A1 WO2008065829 A1 WO 2008065829A1
Authority
WO
WIPO (PCT)
Prior art keywords
gas
molten silicon
container
trichlorosilane
silicon
Prior art date
Application number
PCT/JP2007/070446
Other languages
English (en)
Japanese (ja)
Inventor
Toshiyuki Ishii
Original Assignee
Mitsubishi Materials Corporation
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Mitsubishi Materials Corporation filed Critical Mitsubishi Materials Corporation
Publication of WO2008065829A1 publication Critical patent/WO2008065829A1/fr

Links

Classifications

    • 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
    • C01B33/08—Compounds containing halogen
    • C01B33/107—Halogenated silanes
    • C01B33/1071—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof
    • C01B33/10742—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by hydrochlorination of silicon or of a silicon-containing material
    • C01B33/10757—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by hydrochlorination of silicon or of a silicon-containing material with the preferential formation of trichlorosilane
    • C01B33/10763—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by hydrochlorination of silicon or of a silicon-containing material with the preferential formation of trichlorosilane from silicon
    • 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
    • C01B33/08—Compounds containing halogen
    • C01B33/107—Halogenated silanes
    • C01B33/1071—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof

Definitions

  • the present invention relates to conversion of tetrachlorosilane to trichlorosilane.
  • SiHCl 3 is converted by reacting tetrachlorosilane (SiCl: silicon tetrachloride) with hydrogen.
  • Patent Document 1 tetrachlorosilane and hydrogen are added to a heating element formed of graphite, silicon, or silicon carbide.
  • a technique for spraying a feed gas containing it into trichlorosilane is disclosed. In this manufacturing technology, the sprayed supply gas comes into contact with the heating element, and is heated to obtain a reaction product gas containing trichlorosilane by a conversion reaction.
  • a reaction product gas is obtained by blowing a supply gas onto a heating element formed of graphite, silicon or silicon carbide.
  • the inner wall of the heating element Since it is heating for a short time when it comes into contact with the substrate, there is a disadvantage that it is difficult to improve the conversion rate to trichlorosilane, which has a very high thermal efficiency.
  • carbon, hydrogen, chlorosilane, and hydrogen chloride in the supply gas and reaction product gas react to produce methane, methylchlorosilane, silicon carbide, etc., and impurities. There was an inconvenience.
  • Patent Document 1 JP-A 53-97996
  • the present invention has been made in view of the above-described problems, and provides a trichlorosilane production apparatus capable of improving the conversion rate with high thermal efficiency and further preventing the generation of impurities. With the goal.
  • the present invention employs the following configuration in order to solve the above-described problems. That is, the trichlorosilane manufacturing apparatus of the present invention blows a supply gas containing a container for storing molten silicon, a heating mechanism for heating the molten silicon in the container, and tetrachlorosilane and hydrogen into the molten silicon. A gas supply unit.
  • This trichlorosilane manufacturing apparatus includes a gas supply unit that blows out a supply gas containing tetrachlorosilane and hydrogen into molten silicon. For this reason, the supply gas is released in the form of bubbles in the heated high-temperature molten silicon, whereby it is efficiently heated and undergoes a conversion reaction, and trichlorosilane is obtained with a high conversion rate. Also, silicon is generated from the trichlorosilane in the generated reaction gas by a reduction reaction and a thermal decomposition reaction, and this silicon dissolves into the molten silicon, so that the molten silicon can be increased.
  • the container is formed of quartz
  • the gas supply unit includes a quartz nozzle that inserts a tip into the molten silicon and blows out the supply gas. May be.
  • this trichlorosilane production apparatus uses quartz
  • the (SiO 2) nozzle is inserted into the molten silicon in the quartz container, and the supply gas is
  • the quartz container a crucible used for pulling and generating single crystal silicon can be suitably used.
  • the gas supply unit may be provided with a preheating mechanism for heating the supply gas before blowing it into the molten silicon.
  • a preheating mechanism for heating the supply gas before blowing it into the molten silicon.
  • a gas recovery mechanism for deriving a reaction product gas containing trichlorosilane and hydrogen chloride generated from the supply gas in the molten silicon to the outside from a gas outlet port disposed in an upper portion of the container is provided. It may be.
  • this trichlorosilane production apparatus is equipped with a gas recovery mechanism that leads to the outside from the gas outlet arranged in the upper part of the container, the reaction product gas released from the molten silicon is supplied to the gas outlet in the upper part of the container. Can be collected efficiently.
  • a support member may be provided to support the outer surface of the container so as to cover it.
  • the support member supports the outer surface of the container so that even if the quartz container is softened at a high temperature, the support member supports the container from the surroundings so that the container is supported from the surroundings. Shape change and the like can be prevented.
  • the trichlorosilane production apparatus includes a gas supply unit that blows out a supply gas containing tetrachlorosilane and hydrogen into the molten silicon! /, So that the supply in a bubble state in the molten silicon is provided.
  • Trichlorosilane can be obtained at a high conversion rate by being heated efficiently by contact between the gas and molten silicon.
  • the silicon produced by the reduction reaction and thermal decomposition reaction from a part of the trichlorosilane in the reaction gas is dissolved in the molten silicon, so that it is possible to increase the amount of molten silicon.
  • FIG. 1 is a simplified cross-sectional view showing an embodiment of a trichlorosilane production apparatus according to the present invention.
  • the trichlorosilane production apparatus of the present embodiment includes a quartz (SiO 2) container 1 that stores molten silicon S, and a heating mechanism 2 that heats molten silicon S in the container 1. , Te
  • the container 1 uses a quartz crucible used for pulling and generating single crystal silicon, and the inner bottom surface is formed into an arcuate concave surface la and the arcuate concave surface la is used. A continuous cylindrical inner surface lb is formed at the top.
  • the gas supply unit 3 includes a quartz nozzle 6 whose tip is inserted into the molten silicon S and blows out the supply gas, and a pressure pump P1 connected to the quartz nozzle 6 to supply the supply gas under pressure P1 And a supply source (not shown) of a supply gas connected to the pressure pump P1, and a preheating mechanism 11 for heating the supply gas before blowing it into the molten silicon S.
  • the quartz nozzle 6 is inserted vertically upward from the top of the container 1, and a plurality of outlets 6 b are formed in the end plate 6 a that closes the tip of the quartz nozzle 6.
  • the supply gas is blown into the molten silicon S from the port 6b.
  • the supply gas blown out is dispersed as bubbles in the molten silicon S.
  • the quartz nozzle 6 On the outside of the quartz nozzle 6, there is an outer cylinder member 8 arranged coaxially with the quartz nozzle 6. It is fixed to the top of the container 1. A space between the quartz nozzle 6 and the outer cylinder member 8 serves as a reaction product gas outlet channel, and the lower end opening serves as the gas outlet port 4. That is, the quartz nozzle 6 and the outer cylinder member 8 have a double tube structure. In this case, the outer cylinder member 8 is fixed to the upper end portion of the container 1 via the ring-shaped closing member 12.
  • the gas recovery mechanism 5 is provided with an exhaust pump P2 connected to the gas outlet 4 and sucking the reaction product gas! /, When the reaction product gas can be discharged by a pressure difference The exhaust pump can be omitted.
  • the quartz container 1 is supported by a carbon support member 7 so as to cover the outer surface thereof.
  • the carbon support member 7 includes a support portion body 7a having an inner surface that houses the container 1 and contacts the entire outer surface thereof, and a support column portion 7b provided at a lower portion of the support portion body 7a. It is equipped with.
  • the heating mechanism 2 includes a heater part 2a that is a heat generating part disposed around the container 1 so as to surround the container 1, and an electrode that is connected to a lower part of the heater part 2a and allows a current to flow through the heater part 2a.
  • the portion 2b and an annular bottom heater portion 9 disposed below the container 1 are provided.
  • the electrode portion 2b is connected to a power source (not shown).
  • the bottom heater portion 9 is installed below the support portion main body 7a in a state where the support column portion 7b of the carbon support member 7 is passed through. In addition, the bottom heater unit 9 is also not shown in FIG.
  • the heating mechanism 2 performs heating control so that the molten silicon S in the container 1 has a melting temperature of 1420 ° C. Since the feed gas is heated to 1200 ° C or higher, the conversion rate is improved. Further, disilanes may be introduced into the supply gas and the silanes may be taken out.
  • a supply gas containing tetrachlorosilane and hydrogen is melted with silicon. Since the gas supply unit 3 that blows out into the gas S is provided, the supply gas is released in the form of bubbles into the heated high-temperature molten silicon S. Trichlorosilane is obtained at a high rate. In addition, silicon is generated from the trichlorosilane in the generated reaction gas by a reduction reaction and a thermal decomposition reaction, and this silicon dissolves into the molten silicon S. Therefore, the molten silicon S can be increased.
  • the gas recovery mechanism 5 that leads to the outside from the gas outlet 4 disposed in the upper part of the container 1 is provided, the reaction product gas released from the molten silicon S is supplied to the gas outlet in the upper part of the container 1. It can be efficiently recovered from 4.
  • the periphery of the container 1 is supported by the carbon support member 7, even if the quartz container 1 is softened at a high temperature, the container 1 is supported by the carbon support member 7 from the periphery. It is possible to prevent changes in the shape and the like.
  • the molten silicon S is heated by other methods such as a force S for heating the molten silicon S in the container 1 by radiant heat from the heater 2a, high-frequency induction heating, and the like. It doesn't matter.
  • a force S using one quartz nozzle 6 and a plurality of quartz nozzles 6 may be employed.
  • the outlet is formed in the end plate.
  • the supply gas may be directly blown out from the nozzle opening by reducing the diameter of each nozzle.
  • trichlorosilane can be obtained with a high conversion rate.
  • silicon generated by a reduction reaction and thermal decomposition reaction from a part of trichlorosilane in the generated reaction gas dissolves in the molten silicon, it is possible to increase the molten silicon. For this reason, it is used as a raw material for producing high-purity silicon.
  • C which can be suitably used in the production process of trichlorosilane

Abstract

La présente invention concerne un dispositif de production de trichlorosilane, comprenant une cuve destinée à retenir le silicium fondu, un mécanisme de chauffage permettant le chauffage du silicium fondu retenu dans la cuve et une unité d'alimentation en gaz permettant d'insuffler un gaz comprenant du tétrachlorosilane et de l'hydrogène dans le silicium fondu.
PCT/JP2007/070446 2006-11-30 2007-10-19 Dispositif de production de trichlorosilane WO2008065829A1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
JP2006323693 2006-11-30
JP2006-323693 2006-11-30
JP2007-249627 2007-09-26
JP2007249627 2007-09-26

Publications (1)

Publication Number Publication Date
WO2008065829A1 true WO2008065829A1 (fr) 2008-06-05

Family

ID=39467626

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP2007/070446 WO2008065829A1 (fr) 2006-11-30 2007-10-19 Dispositif de production de trichlorosilane

Country Status (2)

Country Link
JP (1) JP2009096678A (fr)
WO (1) WO2008065829A1 (fr)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5535679B2 (ja) * 2010-02-18 2014-07-02 株式会社トクヤマ トリクロロシランの製造方法
CN102795628B (zh) * 2012-08-03 2014-01-15 东华工程科技股份有限公司 一种改进的低压合成工艺制备三氯氢硅的方法

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH07232910A (ja) * 1994-01-28 1995-09-05 Hemlock Semiconductor Corp テトラクロロシランの水素添加法
JPH1029813A (ja) * 1995-12-25 1998-02-03 Tokuyama Corp トリクロロシランの製造方法
JP2003020217A (ja) * 2001-07-03 2003-01-24 Tokuyama Corp シリコンおよびトリクロロシランの製造法

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH07232910A (ja) * 1994-01-28 1995-09-05 Hemlock Semiconductor Corp テトラクロロシランの水素添加法
JPH1029813A (ja) * 1995-12-25 1998-02-03 Tokuyama Corp トリクロロシランの製造方法
JP2003020217A (ja) * 2001-07-03 2003-01-24 Tokuyama Corp シリコンおよびトリクロロシランの製造法

Also Published As

Publication number Publication date
JP2009096678A (ja) 2009-05-07

Similar Documents

Publication Publication Date Title
JP5119856B2 (ja) トリクロロシラン製造装置
JP3518869B2 (ja) 発熱反応を利用したポリシリコンの調製方法
JP2012501949A (ja) 流動層反応器、その使用及びクロロシランのエネルギー自立型の水素化方法
JPS6261530B2 (fr)
JPS62123011A (ja) トリクロルシランの製造方法およびその装置
WO2008065829A1 (fr) Dispositif de production de trichlorosilane
JP3958092B2 (ja) シリコン生成用反応装置
CN107074561B (zh) 使用高效混合式水平反应器的多晶硅制造装置和方法
JP4805155B2 (ja) シリコン製造装置
JP2008037735A (ja) シリコン製造装置
WO2008066027A1 (fr) Appareil de fabrication de trichlorosilane
WO2008062629A1 (fr) Appareil pour la fabrication de trichlorosilane
CN102060298B (zh) 一种多晶硅生产装置及多晶硅生产方法
JP2008150273A (ja) トリクロロシラン製造装置
JP2003002628A (ja) シリコン製造装置および製造方法
JP2003020216A (ja) シリコンの製造方法
CN106458607B (zh) 使用卧式反应器制造多晶硅的装置以及该多晶硅的制造方法
JP5160181B2 (ja) トリクロロシラン製造装置
JP4099322B2 (ja) シリコンの製造方法
KR101952731B1 (ko) 수평형 반응기를 이용한 폴리실리콘 제조 장치 및 제조 방법
JPH01100011A (ja) トリクロロシランの工業的製造方法
JP2008037747A (ja) ソーラーグレードのシリコン製造法
US9059220B2 (en) Polysilicon manufacturing device
JP5730423B2 (ja) 熱プラズマ処理装置
JP5502650B2 (ja) ポリシリコンの製造方法

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 07830180

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 07830180

Country of ref document: EP

Kind code of ref document: A1