WO2010087003A1 - Dispositif de production de chaleur - Google Patents

Dispositif de production de chaleur Download PDF

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Publication number
WO2010087003A1
WO2010087003A1 PCT/JP2009/051613 JP2009051613W WO2010087003A1 WO 2010087003 A1 WO2010087003 A1 WO 2010087003A1 JP 2009051613 W JP2009051613 W JP 2009051613W WO 2010087003 A1 WO2010087003 A1 WO 2010087003A1
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WO
WIPO (PCT)
Prior art keywords
terminal
heat generating
carbon
metal terminal
heating
Prior art date
Application number
PCT/JP2009/051613
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English (en)
Japanese (ja)
Inventor
靖史 松尾
晃一 竹村
Original Assignee
電気化学工業株式会社
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 電気化学工業株式会社 filed Critical 電気化学工業株式会社
Priority to JP2010548331A priority Critical patent/JP5436454B2/ja
Priority to PCT/JP2009/051613 priority patent/WO2010087003A1/fr
Priority to TW099102346A priority patent/TW201034955A/zh
Publication of WO2010087003A1 publication Critical patent/WO2010087003A1/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
    • C01B33/08—Compounds containing halogen
    • C01B33/107—Halogenated silanes
    • C01B33/1071—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00—Ohmic-resistance heating
    • H05B3/40—Heating elements having the shape of rods or tubes
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B2203/00—Aspects relating to Ohmic resistive heating covered by group H05B3/00
    • H05B2203/022—Heaters specially adapted for heating gaseous material

Definitions

  • the present invention relates to a heat generating device.
  • the present invention relates to a heat generating apparatus in a trichlorosilane production apparatus that converts tetrachlorosilane and hydrogen into trichlorosilane and a reaction tower using the same.
  • Trichlorosilane is expected to increase in demand as a raw material gas for high-purity silicon used in elements such as semiconductors and solar cells, and there has been a demand for efficient production of these.
  • trichlorosilane used as a raw material for producing high-purity silicon (Si: silicon) is converted by reacting tetrachlorosilane (SiCl 4 : silicon tetrachloride) with hydrogen. Manufactured by.
  • trichlorosilane is produced by a conversion reaction according to the following reaction formula (1).
  • SiCl 4 + H 2 ⁇ SiHCl 3 + HCl (1) This reaction is performed by heating a raw material gas consisting of tetrachlorosilane and hydrogen gasified in a carbon reaction vessel to about 800 ° C. to about 1300 ° C. And in order to improve the conversion rate to a trichlorosilane, the product gas of Reaction formula (1) is rapidly cooled.
  • the target silicon is produced by the reduction reaction and thermal decomposition reaction of trichlorosilane according to the following reaction formulas (2) and (3).
  • Patent Document 1 discloses a chlorosilane and hydrogen reaction vessel in which a reaction chamber surrounded by a heating element includes an outer chamber and an inner chamber formed by two concentric tubes.
  • a supply gas of hydrogen and tetrachlorosilane is supplied from the lower part of the reaction chamber via a heat exchanger provided in the lower part of the reaction chamber, and the product gas after the reaction is discharged from the lower part of the reaction chamber.
  • a reaction vessel has been proposed.
  • Patent Document 2 discloses a reaction vessel in which a feed gas of tetrachlorosilane and hydrogen is supplied to the inside and a reaction product gas of trichlorosilane and hydrogen chloride is generated by a conversion reaction, and is arranged around the reaction vessel.
  • Production of trichlorosilane mainly comprising a heating mechanism for heating the reaction vessel, a heat insulating material arranged to cover the reaction vessel and the surroundings of the heating mechanism, and a storage vessel for storing the reaction vessel, the heating mechanism and the heat insulating material
  • An apparatus is disclosed.
  • An object of the present invention is to provide a heat generating device capable of efficiently cooling the terminal portion of the heat generating device and suppressing corrosion and breakage of the component parts.
  • the heating element includes a pair of heating elements, the heating element having a substantially cylindrical metal terminal, a substantially cylindrical carbon terminal, and a substantially cylindrical heating part, and a lower end of the metal terminal and the carbon terminal.
  • the upper end is connected, the lower end of the carbon terminal and the upper end of the heat generating part are connected, the metal terminal has a water passage inside, and a gas containing tetrachlorosilane and hydrogen is supplied to the inside, so that trichlorosilane and chloride are supplied.
  • a heating device is provided for heating a reaction vessel in which a gas containing hydrogen is produced.
  • the terminal portion can be efficiently cooled, and damage to the components can be suppressed.
  • FIG. 1 Schematic diagram of a heating device according to an embodiment of the present invention Schematic longitudinal cross-sectional view of the terminal part of the heat generating apparatus which concerns on embodiment of this invention Schematic longitudinal cross-sectional view of the terminal part of the heat generating apparatus which concerns on embodiment of this invention Schematic of a tetrachlorosilane reaction tower using a heating device according to an embodiment of the present invention
  • Heat generating device 2 Heat generating element 3: Metal terminal 4: Carbon terminal 5: Heat generating portion 6: Water passage 7: Connection portion 8: Male screw portion 9: Female screw portion 10: Inlet 11: Discharge port 12: Water passage Bottom 13: injection tube 14: reaction tower 15: reaction vessel 16: outer cylinder 17: gas inlet 18: reaction product gas outlet
  • the heat generating apparatus 1 includes a reaction vessel in which a gas containing tetrachlorosilane and hydrogen is supplied to generate a gas containing trichlorosilane and hydrogen chloride.
  • a heating device 1 for heating wherein the heating device 1 includes a pair of heating elements 2, and the heating element 2 has a substantially cylindrical metal terminal 3, a substantially cylindrical carbon terminal 4, and a substantially cylindrical heat generation.
  • a lower end portion of the metal terminal 3 and an upper end portion of the carbon terminal 4 are connected, a lower end portion of the carbon terminal 4 and an upper end portion of the heat generating portion 5 are connected, and the metal terminal 3 is It has a water passage 6 inside thereof.
  • the heat generating apparatus 1 having the above-described configuration is provided with a characteristic water passage 6 inside the metal terminal 3 so that the terminal can be connected even at a high temperature of about 800 ° C. to about 1300 ° C., for example.
  • the portion can be efficiently cooled, and corrosion and breakage of the component parts can be suppressed.
  • the metal terminal 3 typically has a substantially cylindrical outer diameter from the heat-resistant surface, as in the case of conventionally used ones.
  • the shape of the metal terminal 3 is not specifically limited, For example, a rectangular parallelepiped shape etc. may be sufficient.
  • alloy materials such as SUS material which has heat resistance and SCC (stress corrosion cracking) resistance.
  • SUS material which has heat resistance and SCC (stress corrosion cracking) resistance.
  • SCC stress corrosion cracking
  • an alloy having high SCC resistance such as Inconel 600 is preferable.
  • the lower end portion of the metal terminal 3 is connected to the upper end portion of the carbon terminal 4 described later.
  • a connecting means (connecting portion 7) for connecting the carbon terminal 4 is provided at the lower end portion of the metal terminal 3.
  • the metal terminal 3 has a male screw portion 8
  • the carbon terminal 4 has a female screw portion 9
  • the metal terminal 3 and the carbon terminal. 4 is preferably configured to be screwed together in the male screw portion 8 and the female screw portion 9.
  • the metal terminal 3 has a water passage 6 provided therein.
  • the water passage 6 is for circulating cooling water for cooling the metal terminal 3, and as shown in FIG. 2 or 3, the inside of the substantially cylindrical metal terminal 3 is arranged in the axial direction.
  • a cavity formed along the cavity, and an inlet 10 and an outlet 11 for cooling water following the cavity are provided.
  • the shape of the water flow path 6 is not specifically limited, It is preferable that it is a cylindrical cavity shape which can circulate cooling water efficiently.
  • the water passage 6 may be simply a metal terminal 3 provided with an inlet 10 and an outlet 11, but as shown in FIG. 2 or 3, the bottom of the water passage of the water passage 6. 12 is preferably provided with a cooling water injection pipe 13 that reaches 12.
  • the cooling water flows into the lower end of the water passage 6 through the injection pipe 13 and is discharged from the upper discharge port 11.
  • the cooling water circulates efficiently and can be cooled effectively.
  • the depth of the water passage 6 that is, the position where the water passage 6 is formed at the lower end of the metal terminal 3, the bottom 12 of the water passage 6 of the water passage 6 is, as shown in FIG. It is preferable to be at a position reaching the screw portion 8.
  • the connecting portion can be efficiently cooled, so that the corrosion of the connecting portion between the metal terminal 3 and the carbon terminal 4 is effectively suppressed. can do.
  • the depth of the water passage 6 is preferably formed to a depth of 100%, more preferably 150% of the formation width of the male screw portion 8.
  • the depth of the water passage 6 may be, for example, such that the bottom portion 12 of the water passage is above the male screw portion 8 at the lower end of the metal terminal 3 as shown in FIG.
  • the diameter of the water passage 6 is not particularly limited as long as the metal terminal 3 is designed so that sufficient strength can be maintained, but may be in a range of 20% to 70% of the diameter of the metal terminal 3. preferable. In particular, if the diameter of the water passage 6 is 30% to 50% of the diameter of the metal terminal 3, the effect of increasing the water flow velocity and increasing the overall heat transfer coefficient can be obtained. Moreover, as shown in FIG. 2, it is preferable that the diameter of the water flow path 6 becomes small according to the diameter in the external thread part 8 of the lower end part of the metal terminal 3 part. Thus, by defining the diameter of the water passage 6 in accordance with the outer diameter of the metal terminal 3, cooling can be performed more effectively.
  • a cooling liquid such as a calcium chloride aqueous solution, an ethylene glycol aqueous solution, or a propylene glycol aqueous solution, or a cooling gas such as cooling nitrogen may be flowed.
  • the carbon terminal 4 is connected to the lower end portion of the metal terminal 3 at the upper end portion thereof, and is connected to the upper end portion of the heat generating portion 5 described later at the lower end portion thereof.
  • Such a carbon terminal 4 is interposed between the metal terminal 3 and the heat generating portion 5, and the metal terminal 3 and the carbon terminal 4 are cooled to cause damage when a carbon heating element is directly connected to the metal terminal. Can be prevented.
  • the diameter of the carbon terminal 4 is preferably larger than the diameter of the metal terminal 3 or the heat generating part 5. Thereby, the effect of reducing the calorific value can be obtained.
  • the diameter of the carbon terminal 4 is preferably 1 to 2 times that of the metal terminal 3 and the heat generating portion 5. Since the diameter of the carbon terminal 4 is 1 to 2 times that of the metal terminal 3 or the heat generating portion 5, the effect of reducing the amount of heat generated can be obtained.
  • the heat generating portion 5 is connected to the lower end portion of the carbon terminal 4 at the upper end portion thereof.
  • the heat generating portion 5 and the carbon terminal 4 are preferably screwed together by, for example, a screw thread.
  • the carbon of the carbon terminal 4 and / or the heat generating part 5 is preferably graphite.
  • the effect of improving heat resistance can be obtained by using graphite.
  • the silicon carbide film is not particularly limited, but typically can be formed by vapor deposition by a CVD method.
  • a mixed gas of a silicon halide compound such as tetrachlorosilane or trichlorosilane and a hydrocarbon compound such as methane or propane is used.
  • Method of use or heated carbon terminal 4 and heat generation while pyrolyzing a silicon halide compound having a hydrocarbon group such as methyltrichlorosilane, triphenylchlorosilane, methyldichlorosilane, dimethyldichlorosilane, trimethylchlorosilane with hydrogen A method of depositing silicon carbide on the surface of the portion 5 can be used.
  • the thickness of the silicon carbide coating is preferably 10 to 500 ⁇ m, more preferably 30 to 300 ⁇ m. If the thickness of the silicon carbide coating is 10 ⁇ m or more, the corrosion of the carbon terminal 4 and the heat generating part 5 due to high-temperature water in the air can be sufficiently suppressed, and if it is 500 ⁇ m or less, the silicon carbide coating is cracked. Further, cracking of the carbon terminal 4 and the heat generating portion 5 is not promoted.
  • the formed silicon carbide coating is a dense and uniform pinhole-free coating and is excellent in chemical stability. Therefore, in the heating device 1 constituted by the carbon terminal 4 and the heating section 5 provided with the silicon carbide coating, The frequency of equipment repair can be reduced, and the work efficiency can be further improved.
  • the reaction tower 14 provided with the heat generating apparatus 1 according to the present embodiment will be described.
  • the reaction tower 14 is supplied with a gas containing tetrachlorosilane and hydrogen, and heats the reaction vessel 15 in which a gas containing trichlorosilane and hydrogen chloride is generated.
  • the heat generating device 1 is mainly composed of a reaction vessel 15 and an outer tube container 16 disposed so as to surround the heat generating device 1.
  • the reaction vessel 15 is a substantially cylindrical vessel for reacting tetrachlorosilane and hydrogen in a high temperature environment.
  • This container has a gas inlet 17 for taking in tetrachlorosilane as a raw material and hydrogen gas, and a reaction product gas outlet 18 for deriving a reaction product gas containing trichlorosilane and hydrogen chloride.
  • the gas inlet 17 is provided at the bottom of the reaction vessel and the reaction product gas outlet 18 is provided above the reaction vessel 15, but these positions are limited to this. It is not a thing.
  • a plurality of the heating devices 1 are installed with a predetermined interval between the reaction vessel 15 in the reaction tower 14 and the outer cylinder vessel 16.
  • the heat generating apparatus 1 is installed in a state of being suspended from the reaction tower 14 as shown in FIG.
  • the installation method of the heat generating device is not limited to the hanging type as described above.
  • the heat generating device may be installed substantially vertically at the bottom of the reaction tower with the electrode on the lower side.
  • the outer cylinder container 16 is a substantially cylindrical container having an outer side made of a metal such as stainless steel and a carbon panel or a refractory brick arranged on the inner side.
  • the outer cylinder container 16 has a heat insulating performance and has a role of keeping the heat from the heat generating device 1 inside and maintaining the temperature in the reaction container 15.
  • the reaction vessel 15 is heated by the heating device 1 disposed around it, so that tetrachlorosilane and hydrogen gas introduced from the gas introduction port 17 of the reaction vessel 15 have a high temperature of about 800 ° C. to about 1300 ° C. And is extracted from the reaction product gas outlet 18 of the reaction vessel 15 in the form of a reaction product gas containing trichlorosilane. Thereafter, the reaction product gas is supplied to a cooling device or the like in order to separate trichlorosilane.
  • the heat generating device 1 includes a pair of heat generating elements, and the heat generating element includes a substantially cylindrical metal terminal, a substantially cylindrical carbon terminal, and a substantially cylindrical heat generating portion, and a lower end portion of the metal terminal. And the upper end of the carbon terminal are connected, the lower end of the carbon terminal and the upper end of the heat generating part are connected, the metal terminal has a water passage inside, and a gas containing tetrachlorosilane and hydrogen is supplied to the inside. It is a heat generating device for heating a reaction vessel in which a gas containing trichlorosilane and hydrogen chloride is generated. According to the heat generating device 1 having the above configuration, since the metal terminal 3 has the water passage 6, the terminal portion including the metal terminal 3 and the carbon terminal 4 can be efficiently cooled, and the heat of the component parts Damage due to expansion can be suppressed.
  • the metal terminal 3 has a male screw portion 8 in the connecting portion 7 where the lower end portion of the metal terminal 3 and the upper end portion of the carbon terminal 4 are connected, and the carbon terminal 4 is
  • the metal terminal 3 and the carbon terminal 4 have a female screw part 9, and the metal terminal 3 and the carbon terminal 4 can be removed and replaced by being screwed together in the male screw part 8 and the female screw part 9. It can be done easily.
  • the diameter of the carbon terminal 4 is 1 to 2 times that of the metal terminal 3 or the heat generating portion 5, an effect of reducing the amount of heat generated can be obtained.
  • the surface of the carbon terminal 4 and the heat generating part 5 can be protected from corrosion by applying a silicon carbide coating on the carbon terminal 4 and / or the heat generating part 5.
  • the silicon carbide film is a silicon carbide film having a thickness of 10 ⁇ m to 500 ⁇ m formed by a CVD method, so that the carbon terminal 4 and heat generated by water in the air at a high temperature or the like are generated.
  • the corrosion of the portion 5 can be sufficiently suppressed, and the crack of the silicon carbide film and the crack of the carbon terminal 4 and the heat generating portion 5 are not promoted.
  • the heat generating device 1 when the carbon of the carbon terminal 4 and / or the heat generating part 5 is graphite, an effect of improving heat resistance can be obtained.
  • a reaction vessel 15 in which a gas containing tetrachlorosilane and hydrogen is supplied to generate a gas containing trichlorosilane and hydrogen chloride, and the heating device 1 arranged so as to surround the reaction vessel 15,
  • the metal terminal 3 has the water passage 6, so the metal terminal 3 and the carbon terminal 4 can be efficiently cooled, and damage due to thermal expansion of components can be suppressed.
  • Example 1 A heating device using a metal terminal provided with a water passage as shown in FIG. 3 was prepared. As shown in FIG. 1, the heat generating device was made into a pair by combining two heat generating elements composed of a metal terminal (diameter 30 mm), a carbon terminal (diameter 30 mm), and a heat generating portion (diameter 20 mm). The diameter of the water passage was 50% of the diameter of the metal terminal. The connecting portion of each member is provided with a screw connection means and connected to each other.
  • the heating device was installed inside the reaction tower and continuously operated for 2000 hours, and then the device was disassembled and examined for damage to the terminal portion. Furthermore, the operation was possible for 2000 hours.
  • Example 2 In Example 2, the carbon terminal and the heat generating part are the same as those in Example 1, but as shown in FIG. 2, only a metal terminal that is deepened only in the depth of the water passage to reach the connecting part is used. A heating device similar to that in Example 1 was prepared except that the above was used. Then, an experiment similar to that in Example 1 was performed, and the device was disassembled to examine the damage of the terminal portion. As a result, the terminal portion was hardly damaged, and the operation for 2000 hours was possible three times.
  • Example 3 In Example 3, the carbon terminal and the heat generating part are the same as those in Example 1, but the same as in Example 1 except that a metal terminal having a water passage diameter 1.5 times that of Example 1 was used. A heating device was created. Then, an experiment similar to that in Example 1 was performed, and the device was disassembled to examine the damage of the terminal portion. As a result, the terminal portion was hardly damaged, and the operation for 2000 hours was possible three times.
  • Example 4 In Example 4, a heat generating device was created using the metal terminal and heat generating part of Example 2 and a carbon terminal (diameter 40 mm) having a diameter larger than that of the metal terminal. Then, an experiment similar to that in Example 1 was conducted, and the device was disassembled to examine the damage of the terminal portion. As a result, the terminal portion was hardly damaged, and the operation for 2000 hours was possible five times.
  • Example 1 A heating device similar to that of Example 1 was prepared except that a metal terminal without a water passage was used. However, when the operation was performed, the heat generating device was damaged when 2000 hours had not passed. When dismantled, it was divided near the connection between the carbon terminal and the metal terminal.
  • the terminal portion was hardly damaged and was excellent in durability.
  • the heat generating devices according to Examples 2 to 4 can withstand multiple uses.

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

Abstract

L'invention porte sur un dispositif de production de chaleur qui permet de refroidir de manière efficace une partie de bornier et qui permet de supprimer l'endommagement d'un composant constitutif. Le dispositif de production de chaleur comprend une paire d'éléments chauffants. Les éléments chauffants comprennent une borne métallique essentiellement cylindrique, une borne en carbone essentiellement cylindrique et une partie de production de chaleur essentiellement cylindrique. L'extrémité inférieure de la borne métallique est reliée à l'extrémité supérieure de la borne en carbone. L'extrémité inférieure de la borne en carbone est reliée à l'extrémité supérieure de la partie de production de chaleur. Un passage d'eau est prévu à l'intérieur de la borne métallique. Le dispositif de production de chaleur est utilisé pour le chauffage d'une cuve de réaction dans laquelle un gaz contenant du tétrachlorosilane et de l'hydrogène est introduit pour produire un gaz contenant du trichlorosilane et du chlorure d'hydrogène.
PCT/JP2009/051613 2009-01-30 2009-01-30 Dispositif de production de chaleur WO2010087003A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
JP2010548331A JP5436454B2 (ja) 2009-01-30 2009-01-30 発熱装置
PCT/JP2009/051613 WO2010087003A1 (fr) 2009-01-30 2009-01-30 Dispositif de production de chaleur
TW099102346A TW201034955A (en) 2009-01-30 2010-01-28 Exothermic device

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/JP2009/051613 WO2010087003A1 (fr) 2009-01-30 2009-01-30 Dispositif de production de chaleur

Publications (1)

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WO2010087003A1 true WO2010087003A1 (fr) 2010-08-05

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PCT/JP2009/051613 WO2010087003A1 (fr) 2009-01-30 2009-01-30 Dispositif de production de chaleur

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JP (1) JP5436454B2 (fr)
TW (1) TW201034955A (fr)
WO (1) WO2010087003A1 (fr)

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
JP2004288510A (ja) * 2003-03-24 2004-10-14 Toshiba Ceramics Co Ltd 昇降温ユニット及びこのユニットを用いた昇降温装置
JP2008133175A (ja) * 2006-10-31 2008-06-12 Mitsubishi Materials Corp トリクロロシラン製造装置

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
JP2004288510A (ja) * 2003-03-24 2004-10-14 Toshiba Ceramics Co Ltd 昇降温ユニット及びこのユニットを用いた昇降温装置
JP2008133175A (ja) * 2006-10-31 2008-06-12 Mitsubishi Materials Corp トリクロロシラン製造装置

Also Published As

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JP5436454B2 (ja) 2014-03-05
JPWO2010087003A1 (ja) 2012-07-26
TW201034955A (en) 2010-10-01

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