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WO2008062629A1 - Appareil pour la fabrication de trichlorosilane - Google Patents

Appareil pour la fabrication de trichlorosilane Download PDF

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Publication number
WO2008062629A1
WO2008062629A1 PCT/JP2007/070735 JP2007070735W WO2008062629A1 WO 2008062629 A1 WO2008062629 A1 WO 2008062629A1 JP 2007070735 W JP2007070735 W JP 2007070735W WO 2008062629 A1 WO2008062629 A1 WO 2008062629A1
Authority
WO
WIPO (PCT)
Prior art keywords
reactor
gas
trichlorosilane
concave surface
arc
Prior art date
Legal status (The legal status 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 status listed.)
Ceased
Application number
PCT/JP2007/070735
Other languages
English (en)
Japanese (ja)
Inventor
Toshiyuki Ishii
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Mitsubishi Materials Corp
Original Assignee
Mitsubishi Materials Corp
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
Priority claimed from JP2007249626A external-priority patent/JP2008150273A/ja
Application filed by Mitsubishi Materials Corp filed Critical Mitsubishi Materials Corp
Publication of WO2008062629A1 publication Critical patent/WO2008062629A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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

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 discloses a supply gas containing tetrachlorosilane and hydrogen in a heating element formed of graphite, silicon, or silicon carbide. A technique for spraying and converting to trichlorosilane is disclosed. This production technology has the advantage that the generated trichlorosilane is immediately removed from the heating element, so that no precipitation of trichlorosilane into silicon occurs even in the temperature range above 1100 ° C.
  • a reaction gas is obtained by spraying a supply gas to a heating element formed of graphite, silicon, or silicon carbide.
  • a heating element When a heating element is configured using, the mechanical strength is low at room temperature, and the mechanical strength is greatly reduced at a high temperature by heating. Therefore, a heating element with higher strength is desired.
  • hydrogen, chlorosilane, and hydrogen chloride in the supply gas and reaction product gas react with each other to produce methane, methylchlorosilane, silicon carbide, and the like. There was an inconvenience of becoming an impurity.
  • the heating element is composed of silicon carbide, the force to use sintered silicon carbide or crystal-grown Pure silicon carbide.
  • the former is usually made using boron as a sintering aid.
  • hydrogen in the supply gas reacts with boron contained in silicon carbide at high temperatures to become BH, which makes it brittle. In the latter case
  • Patent Document 1 JP-A 53-97996
  • the present invention has been made in view of the above-described problems, and an object of the present invention is to provide a trichlorosilane production apparatus that has high mechanical strength, prevents generation of impurities, and can suppress increase in member cost. To do.
  • the present invention employs the following configuration in order to solve the above problems.
  • An apparatus for producing trichlorosilane according to the present invention includes a reactor formed of quartz, a heating mechanism for heating the reactor, and a gas blowing mechanism for blowing a supply gas containing tetrachlorosilane and hydrogen to the reactor. /!
  • the reactor to which the feed gas can be blown is made of quartz, so the reactor has high mechanical strength and high purity not only at room temperature but also at high temperatures of 800 ⁇ ; 1400 ° C. Can be formed. Further, it is possible to obtain trichlorosilane having a high purity without causing the reactor to react with gas components in the supply gas and the reaction product gas to generate impurities. In addition, quartz is less expensive than pure silicon carband, so it is possible to suppress the increase in material costs.
  • the reactor has an arc-shaped concave surface, and the gas blowing mechanism injects the supply gas toward the arc-shaped concave surface in the reactor.
  • An injection nozzle may be provided.
  • the supply gas is injected from the injection nozzle toward the arc-shaped concave surface of the reactor, so that the supply gas injected and collided with the reactor flows along the arc of the arc-shaped concave surface.
  • the conversion reaction can be more efficiently performed by the heating effect from the arcuate concave surface.
  • a quartz crucible used for pulling and generating single crystal silicon can be suitably used.
  • a reaction product gas containing trichlorosilane and hydrogen chloride generated from the supply gas in the reactor is disposed inside the peripheral edge of the arcuate concave surface in the reactor.
  • a gas recovery mechanism that leads to the outside from the gas outlet may be provided.
  • the reaction product gas is led out to the outside from the gas outlet port arranged on the inner periphery of the reactor, so that it is generated by colliding with the arcuate concave surface in the reactor. The reaction product gas that flows back along the arc can be efficiently recovered.
  • the trichlorosilane production apparatus of the present invention may include a support member that supports the outer surface of the reactor.
  • the support member since the support member covers the outer surface of the reactor, the support member is supported from the surroundings even if the reactor softens at high temperatures. Changes in the shape of the reactor can be prevented.
  • the reactor for blowing the supply gas is formed of stone, the reactor is not only at room temperature but also at a reaction temperature of 800 to 1400 ° C. It is possible to obtain trichlorosilane having high strength and high purity, which can form a reactor with high purity quartz and does not generate impurities.
  • FIG. 1 is a simplified cross-sectional view showing an embodiment of a trichlorosilane production apparatus according to the present invention.
  • 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 reactor 1 having an arc-shaped concave surface la formed of quartz, a heating mechanism 2 for heating the reactor 1, a tetrachlorosilane and hydrogen.
  • a gas spray mechanism 3 for spraying a feed gas containing 1 to the reactor 1 and a reaction product gas containing trichlorosilane and hydrogen chloride generated from the feed gas in the reactor 1 are arranged inside the periphery of the reactor 1.
  • a gas recovery mechanism 5 that leads out from the gas outlet 4.
  • the reactor 1 uses a quartz crucible used for pulling and generating single crystal silicon, and is arranged with its arcuate concave surface la facing upward, and the arcuate concave surface la force A continuous cylindrical inner surface lb is formed at the top.
  • the gas blowing mechanism 3 includes an injection nozzle 6 that is arranged on the central axis of the upper part of the reactor 1 and that injects the supply gas toward the arcuate concave surface la of the reactor 1. Further, an outer cylinder member 7 arranged coaxially with the injection nozzle 6 is provided on the outer side of the injection nozzle 6, and this outer cylinder member 7 is provided on the inner side of the cylindrical inner surface lb above the reactor 1. Further, it is fixed via a ring-shaped closing member 11. A space between the injection nozzle 6 and the outer cylinder member 7 serves as a reaction product gas outlet channel 8, and a lower end opening serves as a gas outlet 4. That is, the injection nozzle 6 and the outer cylinder member 7 have a double pipe structure. The injection nozzle 6 is arranged so that the tip protrudes from the gas outlet 4 to the inside of the reactor 1.
  • the gas blowing mechanism 3 includes an injection pump P1 connected to the injection nozzle 6 and pressurizing and supplying the supply gas, and includes a preheating mechanism 12 that heats the supply gas before supplying it to the reactor 1.
  • the injection pump P1 is connected to a supply source (not shown) of the supply gas. Yes.
  • the gas recovery mechanism 5 is connected to the gas outlet 4 and is equipped with an exhaust pump P2 that sucks the reaction product gas S. If the reaction product gas can be discharged by a pressure difference, the gas recovery mechanism 5 The pump can be omitted.
  • the quartz reactor 1 is supported at its periphery by a carbon support member 9.
  • the carbon support member 9 includes a support body 9a that covers the periphery of the reactor 1, and a support column 9b that is provided at the lower portion of the support body 9a.
  • the heating mechanism 2 is arranged around the reactor 1 so as to surround the reactor 1, and is connected to the lower part of the heater unit 2a that is a heat generating unit and flows through the heater unit 2a. And an annular bottom heater section 10 disposed below the reactor 1.
  • the electrode portion 2b is connected to a power source (not shown).
  • the bottom heater portion 10 is installed below the support portion main body 9a in a state where the support column portion 9b of the carbon support member 9 is passed through.
  • the bottom heater unit 10 is also connected to an electrode unit (not shown).
  • the heating mechanism 2 performs calorie heat control so that the reactor 1 has a temperature in the range of 800 ° C to 1400 ° C. If reactor 1 is set 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.
  • the reactor 1 to which the supply gas is blown is formed of quartz
  • the reactor 1 has a high mechanical strength not only at room temperature but also at a high temperature of 800 to 1400 ° C.
  • the reactor 1 can be formed of high-purity quartz.
  • the reactor 1 does not react with the gas components in the supply gas and the reaction product gas to generate impurities, and thus high purity trichlorosilane can be obtained.
  • quartz is less expensive than pure silicon carbide, it is possible to suppress an increase in material costs.
  • the supply gas is injected from the injection nozzle 6 toward the arc-shaped concave surface la in the reactor 1, the supply gas that has been injected and collided with the arc-shaped concave surface 1a of the reactor 1 is arc-shaped concave surface 1 a
  • the force S is applied to make the conversion reaction more efficiently by the heating effect from the arcuate concave surface la.
  • reaction product gas is led out from the gas outlet 4 disposed inside the peripheral edge of the reactor 1, it is generated by colliding with the arc-shaped concave surface la of the reactor 1 and from the arc-shaped concave surface la.
  • the reaction product gas that flows back upward along the cylindrical inner surface lb can be efficiently recovered.
  • the carbon support member 9 supports from the periphery, so that the shape of the reactor 1 Changes can be prevented.
  • the heating mechanism 2 may be a power that heats the reactor 1 with radiant heat from the heater 2a.
  • the reactor 1 may be heated by other methods such as high-frequency induction heating.
  • the reactor 1 has a configuration in which the cylindrical inner surface lb is continuously formed from the arc-shaped concave surface la, but at least the surface on which the supply gas is blown may be a circular arc-shaped concave surface. Even if there is no inner surface, the force S can smoothly flow the gas that collides with the arc-shaped concave surface along the surface of the reactor.
  • the arcuate concave surface may not be an arc having the same curvature, but may be a series of arcs having a plurality of curvatures.
  • An arc-shaped concave surface is suitable for recovering the reaction product gas, but in the present invention, a surface shape other than the arc-shaped concave surface is not excluded.
  • the ring-shaped closing member is formed in a tapered plate shape, an arc plate shape, or the like continuous from the cylindrical inner surface. You can do it.
  • the reactor for blowing the supply gas is formed of quartz
  • the reactor has a high mechanical strength even at a reaction temperature of 800 to 1400 ° C
  • the reactor can be formed of high purity quartz. Further, high purity trichlorosilane can be obtained without generating impurities. For this reason, high purity silicon is produced. Therefore, it can be suitably used in the production process of trichlorosilane used as a raw material for the purpose.

Landscapes

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

Abstract

Cette invention porte sur un appareil pour la fabrication du trichlorosilane, comprenant un réacteur formé de quartz, un mécanisme de chauffage pour chauffer le réacteur, et un mécanisme de pulvérisation de gaz pour pulvériser un gaz d'alimentation contenant du tétrachlorosilane et de l'hydrogène contre le réacteur. Le réacteur présente une face renfoncée en forme d'arc, et le mécanisme de pulvérisation de gaz peut comporter une buse à jet pour projeter le gaz d'alimentation vers la face renfoncée en forme d'arc du réacteur.
PCT/JP2007/070735 2006-11-21 2007-10-24 Appareil pour la fabrication de trichlorosilane Ceased WO2008062629A1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
JP2006314897 2006-11-21
JP2006-314897 2006-11-21
JP2007-249626 2007-09-26
JP2007249626A JP2008150273A (ja) 2006-11-21 2007-09-26 トリクロロシラン製造装置

Publications (1)

Publication Number Publication Date
WO2008062629A1 true WO2008062629A1 (fr) 2008-05-29

Family

ID=39429568

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP2007/070735 Ceased WO2008062629A1 (fr) 2006-11-21 2007-10-24 Appareil pour la fabrication de trichlorosilane

Country Status (1)

Country Link
WO (1) WO2008062629A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103153857A (zh) * 2010-08-12 2013-06-12 赢创德固赛有限公司 具有集成式换热器的反应器在将四氯化硅加氢脱氯方法中的应用

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS4847500A (fr) * 1971-10-21 1973-07-05
JPS5397996A (en) * 1977-02-09 1978-08-26 Mitsubishi Metal Corp Production of trichlorosilane
JPS6325211A (ja) * 1986-07-10 1988-02-02 Chiyoda Chem Eng & Constr Co Ltd トリクロロシランの製造方法

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS4847500A (fr) * 1971-10-21 1973-07-05
JPS5397996A (en) * 1977-02-09 1978-08-26 Mitsubishi Metal Corp Production of trichlorosilane
JPS6325211A (ja) * 1986-07-10 1988-02-02 Chiyoda Chem Eng & Constr Co Ltd トリクロロシランの製造方法

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103153857A (zh) * 2010-08-12 2013-06-12 赢创德固赛有限公司 具有集成式换热器的反应器在将四氯化硅加氢脱氯方法中的应用

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