WO2012147300A1 - Dispositif de production de silicium polycristallin et procédé s'y rapportant - Google Patents

Dispositif de production de silicium polycristallin et procédé s'y rapportant Download PDF

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Publication number
WO2012147300A1
WO2012147300A1 PCT/JP2012/002619 JP2012002619W WO2012147300A1 WO 2012147300 A1 WO2012147300 A1 WO 2012147300A1 JP 2012002619 W JP2012002619 W JP 2012002619W WO 2012147300 A1 WO2012147300 A1 WO 2012147300A1
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Prior art keywords
core wire
silicon
polycrystalline silicon
electrode
silicon core
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PCT/JP2012/002619
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English (en)
Japanese (ja)
Inventor
靖志 黒澤
祢津　茂義
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信越化学工業株式会社
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Publication of WO2012147300A1 publication Critical patent/WO2012147300A1/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 technique for producing polycrystalline silicon.
  • Siemens method is known as a method for producing polycrystalline silicon which is a raw material for single crystal silicon for semiconductors or silicon for solar cells.
  • the Siemens method is a method in which a raw material gas containing chlorosilane is brought into contact with a heated silicon core wire, and polycrystalline silicon is vapor-phase grown on the surface of the silicon core wire using a CVD (Chemical Vapor Deposition) method.
  • CVD Chemical Vapor Deposition
  • the reactor for vapor-phase growth of polycrystalline silicon by the Siemens method has two vertical silicon core wires in a space composed of an upper structure called a bell jar and a lower structure called a base plate (bottom plate).
  • One torii type is assembled, and both ends of the torii type silicon core wire are fixed to a pair of metal electrodes disposed on the base plate via a pair of carbon core wire holders.
  • Patent Document 1 Japanese Patent Publication No. 37-18861
  • the electrode passes through the base plate with an insulator in between, and is connected to another electrode through wiring or connected to a power source arranged outside the reactor.
  • a coolant such as water.
  • the electrode and the core wire holder may be joined directly, but a carbon adapter is provided between the electrode and the core wire holder for the purpose of preventing damage to the electrode.
  • a silicon core wire When a silicon core wire is heated to a temperature range of 900 ° C. or higher and 1200 ° C. or lower in a hydrogen atmosphere by passing a current from the electrode, a mixed gas of, for example, trichlorosilane and hydrogen is supplied from a gas nozzle into the reactor as a source gas. Silicon is vapor-grown on the core wire, and a polycrystalline silicon rod having a desired diameter is formed in an inverted U shape.
  • the silicon core wire is made of polycrystalline or single crystal silicon
  • the silicon core wire used for manufacturing high-purity polycrystalline silicon needs to be high-purity with a low impurity concentration, specifically,
  • the specific resistance is required to be high resistance of about 500 ⁇ ⁇ cm or more. Since energization of such a high resistance silicon core wire generally cannot be started at room temperature, it is necessary to energize the silicon core wire in advance by initially heating the silicon core wire to about 200 to 400 ° C. to lower the specific resistance (increasing conductivity). is there.
  • a carbon heater for initial heating is provided at the center or inner peripheral surface of the reaction furnace, and at the start of the reaction, this carbon heater is first heated by energization, and by the radiant heat generated at that time.
  • a silicon core wire disposed around the carbon heater is heated to a desired temperature.
  • the surface temperature of the silicon core wire is adjusted by applying a voltage of 2.0 V / cm to 8.0 V / cm per length to the silicon core wire. It is possible to start energization in the range of 900 ° C. or higher and 1300 ° C. or lower.
  • the surface temperature is maintained by the heat generated by the silicon core wire itself without using heating using a carbon heater, so that the precipitation reaction proceeds continuously. Therefore, after the energization of the silicon core wire is started, the power source of the carbon heater is turned off.
  • the silicon core wire does not reach a sufficient temperature due to the initial heating at the start of the precipitation reaction (at the start of energization), the specific resistance of the silicon core wire does not sufficiently decrease. For this reason, the applied voltage at the start of energization needs to be set higher. However, if the applied voltage is increased, spark discharge is likely to occur between the core wire holder and the silicon core wire, and the silicon core wire is damaged. . Such damage also causes the silicon core wire to collapse during the precipitation reaction.
  • the silicon core wire is heated by radiant heat from the carbon heater, but is radiated from the silicon core wire by convection heat transfer to the surrounding gas and conduction heat transfer to the cooled electrode.
  • the core wire holder and the adapter may be made of low thermal conductivity.
  • carbon is often used for these members from the viewpoint of heat resistance, the amount of impurities contained, cost, etc., and the thermal conductivity of carbon is relatively high at 80 to 180 W / mK.
  • there is a choice of making the core wire holder or adapter longer to increase the distance from the electrode but in this case, there are problems that the cost of the carbon member is increased and the space in the reactor must be increased.
  • the present invention has been made to solve such a problem, and suppresses the degree to which the heat of the silicon core wire heated by the carbon heater is dissipated to the electrode side. To provide a technique for efficiently increasing the temperature of the silicon core wire.
  • the polycrystalline silicon manufacturing apparatus supplies a raw material gas to a silicon core wire heated in a reaction furnace, so
  • a polycrystalline silicon manufacturing apparatus for depositing crystalline silicon comprising: a carbon core wire holder for holding the silicon core wire; and an electrode for energizing the silicon core wire, from the electrode to the silicon core wire
  • the heat insulation sheet is arrange
  • the polycrystalline silicon manufacturing apparatus is for depositing polycrystalline silicon on the surface of the silicon core wire by supplying a raw material gas to the silicon core wire heated in the reactor.
  • a polycrystalline silicon manufacturing apparatus comprising: a carbon core wire holder for holding the silicon core wire; and an electrode for energizing the silicon core wire, and a heat insulating sheet is provided at a contact portion between the silicon core wire and the core wire holder. It is arrange
  • the polycrystalline silicon manufacturing apparatus is for depositing polycrystalline silicon on the surface of the silicon core wire by supplying a raw material gas to the silicon core wire heated in the reaction furnace.
  • a polycrystalline silicon manufacturing apparatus comprising: a carbon core wire holder for holding the silicon core wire; an electrode for energizing the silicon core wire; and a carbon adapter for mounting the core wire holder on the electrode;
  • a heat insulating sheet is disposed in at least one of a contact portion between the silicon core wire and the core wire holder, a contact portion between the core wire holder and the adapter, and a contact portion between the adapter and the electrode, and The thermal conductivity in the thickness direction of the sheet is lower than the thermal conductivity of the core wire holder and the adapter.
  • the thermal conductivity in the thickness direction of the heat insulating sheet is 10 W / mK or less at 25 ° C., more preferably 5 W / mK or less.
  • the electrical resistivity in the thickness direction of the heat insulating sheet is 5000 ⁇ ⁇ m or less at 25 ° C., more preferably 2000 ⁇ ⁇ m or less.
  • the thickness of the heat insulating sheet is 0.1 mm or more and 4.0 mm or less, and more preferably 0.2 mm or more and 1.0 mm or less.
  • the method for producing polycrystalline silicon according to the present invention uses the polycrystalline silicon production apparatus of the present invention to deposit polycrystalline silicon on the surface of the silicon core wire that is energized from the electrode to the silicon core wire and heated to a predetermined temperature. It is characterized by making it.
  • the heat insulating sheet whose thermal conductivity in the thickness direction is lower than the thermal conductivity of the core wire holder is arranged in at least one part of the conductive path from the electrode to the silicon core wire. The degree to which the heat of the silicon core wire is dissipated to the electrode side is suppressed, thereby providing a technique for efficiently increasing the temperature of the silicon core wire at the start of the precipitation reaction (at the start of energization).
  • Siemens method using trichlorosilane as a source gas will be described as an example, but it goes without saying that it can also be used as another source gas such as monosilane or dichlorosilane.
  • FIG. 1 is a schematic sectional view showing an example of the configuration of a reaction furnace 100 for producing polycrystalline silicon according to the present invention.
  • the reactor 100 is an apparatus for obtaining a polycrystalline silicon rod 12 by vapor-depositing polycrystalline silicon on the surface of the silicon core wire 11 by the Siemens method, and is composed of a base plate 5 and a bell jar 1.
  • the base plate 5 is provided with a metal electrode 10 for supplying a current to the silicon core wire 11, a gas nozzle 9 for supplying a process gas such as nitrogen gas, hydrogen gas, trichlorosilane gas, and an exhaust port 8 for exhausting the exhaust gas.
  • the base plate 5 has a refrigerant inlet 6 and an outlet 7 for cooling itself.
  • the bell jar 1 has a refrigerant inlet part 3 and an outlet part 4 for cooling itself, and further has a viewing window 2 for visually confirming the inside from the outside.
  • FIG. 2 is a diagram for explaining an example of an arrangement relationship among the electrode 10, the adapter 14, the core wire holder 13, and the silicon core wire 11 when a heat insulating sheet to be described later is not arranged.
  • the metal electrode 10 has a refrigerant inlet 15 and an outlet 16 for cooling itself, and has a structure on which an adapter 14 can be placed.
  • the core wire holder 13 is fixed to the upper part of the adapter 14, and the silicon core wire 11 is fixed to the core wire holder 13.
  • the adapter 14 and the core wire holder 13 do not need to be provided as separate members, and may be an integrated core wire holder in which the adapter 14 and the core wire holder 13 are a single member.
  • the electrode 10, the adapter 14, the core wire holder 13, and the silicon core wire 11 are required to have a contact area necessary for energization. Moreover, it is necessary to have sufficient strength to hold the polycrystalline silicon rod obtained by the polycrystalline silicon precipitation reaction.
  • FIG. 3 is a diagram for explaining an example of an arrangement relationship of the electrode 10, the adapter 14, the core wire holder 13, and the silicon core wire 11 when a heat insulating sheet is arranged.
  • the polycrystalline silicon manufacturing apparatus of the present invention includes at least a carbon core wire holder 13 that holds the silicon core wire 11 and an electrode 10 for energizing the silicon core wire 11, and reaches from the electrode 10 to the silicon core wire 11.
  • a heat insulating sheet 17 is disposed in at least one part of the conductive path. The heat conductivity in the thickness direction of the heat insulating sheet 17 is lower than the heat conductivity of the core wire holder 13.
  • the heat insulating sheet 17 is provided at the contact portion between the adapter 14 and the electrode 10.
  • FIGS. 4 to 6 an embodiment (FIG. 4) in which a heat insulating sheet 17 is disposed at the contact portion between the core wire holder 13 and the adapter 14, the silicon core wire 11 and the core wire holder 13
  • positioned at the part may be sufficient.
  • the heat insulating sheet 17 may be disposed in at least one of a contact portion between the silicon core wire 11 and the core wire holder 13, a contact portion between the core wire holder 13 and the adapter 14, and a contact portion between the adapter 14 and the electrode 10.
  • the sheet is made of a material having a degree of conductivity necessary for heating the silicon core wire, and is more thermally conductive than the carbon material that is a constituent material of the core wire holder 13 and the adapter 14. If the property is low, it is effective to use this as a heat insulating sheet. That is, by using such a heat insulating sheet 17, heat radiation to the cooled electrode 10 when the silicon core wire 11 is heated is suppressed, while initial heating of the silicon core wire 11 is also efficiently performed. .
  • the heat insulating property and the electrical conductivity of the heat insulating sheet 17 are basically a trade-off.
  • the thermal conductivity in the thickness direction of the sheet is preferably 10 W / mK or less at 25 ° C., more preferably 5 W / mK or less.
  • the electrical resistivity in the thickness direction is preferably 5000 ⁇ ⁇ m or less, more preferably 2000 ⁇ ⁇ m or less at 25 ° C.
  • the preferable thickness of a heat insulation sheet is 0.1 mm or more and 4.0 mm or less, More preferably, it is 0.2 mm or more and 1.0 mm or less. When the heat insulating sheet is too thick, it causes unnecessary energy loss, and when it is too thin, the heat blocking effect may not be sufficiently obtained.
  • the heat insulating sheet 17 is not particularly limited as long as it has a heat conductivity and conductivity as described above, and is a heat resistant material, and a preferable material is a carbon sheet obtained by rolling graphite. Specifically, carbon sheets obtained by heating and rolling acid-treated graphite (for example, those described in JP-A-58-128807 (Patent Document 3) and JP-A-2006-62922 (Patent Document 4)). Etc.). Since such a material has high conductivity in the area direction, it is easy to ensure sufficient conductivity while obtaining a heat insulating effect. In addition, the carbon sheet of such a physical characteristic is marketed, and can be obtained easily.
  • the silicon core wire 11 is energized from the electrode 10 to deposit polycrystalline silicon on the surface of the silicon core wire 11 heated to a predetermined temperature.
  • the silicon core wire 11 is heated to a temperature at which the silicon core wire 11 can be energized by heating the silicon core wire 11 using an external heater (not shown), and when the temperature of the silicon core wire 11 reaches 200 to 400 ° C. 11 is applied with a voltage from the electrode 10, and the temperature of the silicon core wire 11 is set to 900 to 1300 ° C.
  • a mixed gas of trichlorosilane and hydrogen, which is a raw material, is introduced from the raw material nozzle 9 to deposit polycrystalline silicon on the silicon core wire 11, and the reaction is stopped when the polycrystalline silicon has grown to a predetermined size.
  • the heating time of the silicon core wire 11 can be greatly shortened.
  • it is possible to start energization with a relatively low energization start voltage in a limited heating time it is possible to suppress discharge between the silicon core wire 11 and the core wire holder 13 and the like. It is possible to prevent the core wire from falling down.
  • Examples A and B Polycrystalline silicon was grown under the following conditions. First, four silicon core wires of 8 mm square and 1500 mm length were installed in the reaction furnace, the inside of the furnace was in a hydrogen atmosphere, and initial heating was performed for 10 minutes with a carbon heater (110 kW, heater surface temperature 1250 ° C.). Next, the voltage applied to the silicon core wire was gradually increased, the voltage when the current value began to increase was taken as the energization start voltage, and the voltage was adjusted so that a current of 10 A would flow after energization. After 15 minutes from the start of energization, the silicon core wire was taken out, and the depth of scratches generated on the silicon core wire was measured with a surface roughness measuring instrument.
  • Example A A carbon sheet having a thickness of 1 mm and a thermal conductivity of 5 W / mK in the thickness direction was disposed between the electrode and the adapter.
  • Example B A carbon heat insulating sheet having a thickness of 1 mm and a thermal conductivity of 5 W / mK in the thickness direction is disposed between the electrode and the adapter, and 0.2 mm thick heat is further interposed between the core wire holder and the silicon core wire.
  • a carbon sheet having a conductivity of 5 W / mK was disposed.
  • Comparative example a A heat insulating sheet is not installed between the electrode, the adapter, the core wire holder, and the silicon core wire.
  • Examples C and D Two series of silicon core wires of 8 mm square and 1500 mm length were installed in the reactor (total of 8 wires), and under the same conditions as in Examples A and B, initial heating was performed with a carbon heater, and energization was started. Then, silicon deposition reaction was carried out by introducing trichlorosilane and hydrogen gas.
  • Example C A carbon sheet having a thickness of 1 mm and a thermal conductivity of 5 W / mK in the thickness direction was disposed between the electrode and the adapter.
  • Example D A carbon heat insulating sheet having a thickness of 1 mm and a thermal conductivity of 5 W / mK in the thickness direction is disposed between the electrode and the adapter, and 0.4 mm thick heat is further interposed between the core wire holder and the silicon core wire.
  • a carbon sheet having a conductivity of 5 W / mK was disposed.
  • Comparative example b A heat insulating sheet is not installed between the electrode, the adapter, the core wire holder, and the silicon core wire.
  • the present invention suppresses the degree to which the heat of the silicon core wire heated by the carbon heater is dissipated to the electrode side, thereby efficiently increasing the temperature of the silicon core wire at the start of the precipitation reaction (at the start of energization). I will provide a.

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

Abstract

Le dispositif de production de silicium polycristallin ci-décrit comprend au moins un porte-fil à âme (13) en carbone qui maintient un fil à âme de silicium (11), une électrode (10) pour faire passer un courant dans le fil à âme de silicium (11), et une feuille d'isolation thermique (17) placée au moins à un endroit sur le trajet électroconducteur allant de l'électrode (10) au fil à âme de silicium (11). La conductivité thermique dans le sens de l'épaisseur de la feuille d'isolation thermique (17) est inférieure à celle du porte-fil à âme (13). Il est ainsi possible de réduire l'importance du rayonnement de la chaleur du fil à âme de silicium (11) chauffé par un chauffage au carbone en direction de l'électrode (10), et d'élever efficacement la température du fil à âme de silicium (11) au début d'une réaction de dépôt et au début du passage du courant.
PCT/JP2012/002619 2011-04-27 2012-04-16 Dispositif de production de silicium polycristallin et procédé s'y rapportant WO2012147300A1 (fr)

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JP2011-098983 2011-04-27
JP2011098983A JP5653830B2 (ja) 2011-04-27 2011-04-27 多結晶シリコン製造装置および多結晶シリコン製造方法

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2489634A1 (fr) * 2009-10-14 2012-08-22 Shin-Etsu Chemical Co., Ltd. Support de fil de noyau pour la production de silicium polycristallin et procédé pour produire du silicium polycristallin
JP2013018675A (ja) * 2011-07-11 2013-01-31 Shin-Etsu Chemical Co Ltd 多結晶シリコン製造装置
WO2014103939A1 (fr) * 2012-12-27 2014-07-03 株式会社トクヤマ Barreau de silicium polycristallin et son procédé de fabrication
WO2014168116A1 (fr) * 2013-04-10 2014-10-16 株式会社トクヤマ Support d'âme pour fabrication de silicium

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP6513842B2 (ja) * 2018-02-02 2019-05-15 信越化学工業株式会社 多結晶シリコン棒製造用のシリコン芯線および多結晶シリコン棒の製造装置
JP7100192B2 (ja) * 2018-07-27 2022-07-12 ワッカー ケミー アクチエンゲゼルシャフト 多結晶シリコン堆積用電極

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006016243A (ja) * 2004-07-01 2006-01-19 Sumitomo Titanium Corp 多結晶シリコン製造方法およびシード保持電極
JP2006240934A (ja) * 2005-03-04 2006-09-14 Tokuyama Corp 多結晶シリコンの製造装置
WO2011045881A1 (fr) * 2009-10-14 2011-04-21 信越化学工業株式会社 Support de fil de noyau pour la production de silicium polycristallin et procédé pour produire du silicium polycristallin
JP2011195439A (ja) * 2010-03-19 2011-10-06 Wacker Chemie Ag 黒鉛電極

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006016243A (ja) * 2004-07-01 2006-01-19 Sumitomo Titanium Corp 多結晶シリコン製造方法およびシード保持電極
JP2006240934A (ja) * 2005-03-04 2006-09-14 Tokuyama Corp 多結晶シリコンの製造装置
WO2011045881A1 (fr) * 2009-10-14 2011-04-21 信越化学工業株式会社 Support de fil de noyau pour la production de silicium polycristallin et procédé pour produire du silicium polycristallin
JP2011195439A (ja) * 2010-03-19 2011-10-06 Wacker Chemie Ag 黒鉛電極

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2489634A1 (fr) * 2009-10-14 2012-08-22 Shin-Etsu Chemical Co., Ltd. Support de fil de noyau pour la production de silicium polycristallin et procédé pour produire du silicium polycristallin
EP2489634A4 (fr) * 2009-10-14 2014-12-31 Shinetsu Chemical Co Support de fil de noyau pour la production de silicium polycristallin et procédé pour produire du silicium polycristallin
JP2013018675A (ja) * 2011-07-11 2013-01-31 Shin-Etsu Chemical Co Ltd 多結晶シリコン製造装置
WO2014103939A1 (fr) * 2012-12-27 2014-07-03 株式会社トクヤマ Barreau de silicium polycristallin et son procédé de fabrication
JPWO2014103939A1 (ja) * 2012-12-27 2017-01-12 株式会社トクヤマ 多結晶シリコンロッドおよびその製造方法
WO2014168116A1 (fr) * 2013-04-10 2014-10-16 株式会社トクヤマ Support d'âme pour fabrication de silicium

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JP5653830B2 (ja) 2015-01-14

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