WO2005019106A1 - シリコン製造装置 - Google Patents
シリコン製造装置 Download PDFInfo
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- WO2005019106A1 WO2005019106A1 PCT/JP2004/011774 JP2004011774W WO2005019106A1 WO 2005019106 A1 WO2005019106 A1 WO 2005019106A1 JP 2004011774 W JP2004011774 W JP 2004011774W WO 2005019106 A1 WO2005019106 A1 WO 2005019106A1
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- reaction tube
- silicon
- coil
- temperature
- heated
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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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/02—Apparatus characterised by being constructed of material selected for its chemically-resistant properties
-
- 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
- C01B33/029—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition of monosilane
-
- 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
- C01B33/03—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition of silicon halides or halosilanes or reduction thereof with hydrogen as the only reducing agent
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
- C30B11/003—Heating or cooling of the melt or the crystallised material
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/02—Apparatus characterised by their chemically-resistant properties
- B01J2219/0204—Apparatus characterised by their chemically-resistant properties comprising coatings on the surfaces in direct contact with the reactive components
- B01J2219/0218—Apparatus characterised by their chemically-resistant properties comprising coatings on the surfaces in direct contact with the reactive components of ceramic
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/02—Apparatus characterised by their chemically-resistant properties
- B01J2219/0204—Apparatus characterised by their chemically-resistant properties comprising coatings on the surfaces in direct contact with the reactive components
- B01J2219/0227—Apparatus characterised by their chemically-resistant properties comprising coatings on the surfaces in direct contact with the reactive components of graphite
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/02—Apparatus characterised by their chemically-resistant properties
- B01J2219/025—Apparatus characterised by their chemically-resistant properties characterised by the construction materials of the reactor vessel proper
- B01J2219/0272—Graphite
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
- Y10T117/10—Apparatus
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
- Y10T117/10—Apparatus
- Y10T117/1004—Apparatus with means for measuring, testing, or sensing
Definitions
- the present invention relates to a silicon manufacturing apparatus for manufacturing polycrystalline silicon. More specifically, in the present invention, a raw material gas is supplied to a reaction tube heated by a high-frequency heating coil to precipitate silicon on the inner surface of the reaction tube, and at least a part including the lower end of the reaction tube is made of silicon.
- the present invention relates to an apparatus for producing silicon, in which, while being heated to a temperature higher than its melting point, precipitated silicon is dropped and collected into a collecting section provided below a reaction tube.
- Siemens method a method called the Siemens method.
- a silicon rod heated to the deposition temperature of silicon by energization is placed inside a bell jar, and trichlorosilane (SiHCl) or monosilane (SiH ) With a reducing gas such as hydrogen.
- the silicon manufacturing apparatus 100 includes a reaction tube 102, a gas supply port 103 for supplying chlorosilanes and hydrogen, and a high-frequency heating coil 104 installed on the outer periphery of the reaction tube 102 in a closed vessel 111. .
- the reaction tube 102 is heated by electromagnetic waves from the high-frequency heating coil 104 on the outer periphery thereof, and the inner surface of the reaction tube 102 is heated to a temperature at which the temperature is equal to or higher than the melting point of silicon or lower than the melting point of silicon. Then, chlorosilanes supplied from the gas supply port 103 are brought into contact with the inner surface of the heated reaction tube 102 to deposit silicon.
- the silicon melt deposited in a molten state is continuously discharged from the opening of the lower end portion 102a of the reaction tube 102. And collected by the silicon recovery unit 105 installed in the falling direction.
- silicon is once deposited as a solid on the inner surface of the reaction tube 102. Thereafter, the inner surface is heated to a temperature equal to or higher than the melting point of silicon, and part or all of the precipitate is melted and dropped, and is collected by the silicon collecting unit 105 provided in the falling direction.
- a region in the reactor 100 for example, a gap 107 between the reaction tube 102 and the gas supply tube 106, in which deposition of silicon must be prevented, is filled with a sealing gas such as hydrogen. Further, the exhaust gas after the reaction in the reaction tube 102 is discharged to the outside from a gas discharge tube 108 provided in the closed container 111.
- Reference numeral 110 denotes a partition wall made of quartz or the like for shielding the high-frequency heating coil 104 from the reaction gas atmosphere.
- Patent Document 1 JP 2003-2627 A
- Patent Document 2 Japanese Patent Application Laid-Open No. 2002-29726
- the deposited silicon is melted, dropped, and collected by the silicon recovery unit 105 installed below.
- the molten silicon or the like that has flowed down the inner surface of the tube 102 and reached the lower end portion 102a is cooled, and a part thereof is solidified. If the molten silicon is solidified at the lower end 102a in this manner, the silicon lump is formed to extend downward from the tip of the lower end 102a in an icicle-like manner.
- a heat insulating member may be wound around the outer surface of the reaction tube 102 to suppress heat radiation from the reaction tube 102.
- the current heat insulating member it is difficult to ensure sufficient heat insulation at the lower end portion 102a.
- the heat insulating member may be deteriorated. .
- the present invention has been made to solve the above-mentioned problems in the prior art, and an object of the present invention is to recover the precipitated silicon downward by setting the inner surface of the reaction tube to a temperature equal to or higher than the melting point of silicon.
- An object of the present invention is to provide a silicon production apparatus capable of preventing solidification of molten silicon at a lower end of a reaction tube when the liquid is dropped and collected at a lower end of the reaction tube.
- the silicon production apparatus of the present invention comprises: a reaction tube having a carbon material as a base material;
- a gas supply port for supplying chlorosilanes and hydrogen from an upper portion of the reaction tube, and a high-frequency heating coil provided on an outer peripheral side of the reaction tube;
- An apparatus for producing polycrystalline silicon wherein at least a part including a lower end of the reaction tube can be heated to a temperature equal to or higher than the melting point of silicon by the high-frequency heating coil,
- It is characterized by comprising a temperature drop prevention means for preventing a temperature drop at the lower end of the reaction tube during heating by the high frequency heating coil.
- the temperature decrease prevention means prevents the temperature decrease at the lower end of the reaction tube when the reaction tube is heated by the high-frequency heating coil. Therefore, the inner surface of the reaction tube The solidification of the molten silicon at the lower end of the reaction tube can be prevented when the deposited silicon is dropped to the lower collecting part and collected at a temperature equal to or higher than the melting point of silicon.
- the temperature drop prevention means is an infrared radiation device that heats an outer periphery of a lower end portion of the reaction tube with infrared light.
- the inner surface of the reaction tube is heated to a temperature equal to or higher than the melting point of silicon, and the precipitated silicon is dropped into the lower collecting section to be collected. This prevents a temperature drop in the section and prevents solidification of the molten silicon at the lower end of the reaction tube.
- the infrared radiation device an infrared radiation member having a carbon material as a base material, which is provided on an outer peripheral side of a lower end portion of the reaction tube so as to be spaced apart from the lower end portion,
- the high-frequency heating coil may be arranged on the outer peripheral side of the infrared radiation member so as to heat the infrared radiation member.
- the infrared radiation member is installed on the outer peripheral side of the lower end portion of the reaction tube, and the infrared radiation member is simultaneously heated by the high-frequency heating coil that heats the silicon deposition region of the reaction tube.
- the lower end of the tube is sufficiently heated by the infrared radiation of the infrared radiation member, and a temperature drop at the lower end of the reaction tube can be prevented.
- the temperature lowering prevention means has a higher heating strength than a coil formed near the lower end of the high-frequency heating coil and located above the lower end. This is the lower end coil.
- the inner surface of the reaction tube is brought to a temperature equal to or higher than the melting point of silicon, and when the precipitated silicon is dropped and collected in the lower collecting section, the reaction tube is recovered. This prevents the lowering of the temperature at the lower end of the reaction tube and prevents solidification of the molten silicon at the lower end of the reaction tube.
- the lower end side coil is preferably formed with a coil pitch shorter than the coil pitch of the coil above it.
- the lower end side coil is composed of a plurality of coils wound in multiple directions in the diameter increasing direction.
- the lower end of the reaction tube is heated by the high frequency from each coil wound in multiple layers.
- the heating intensity for the part is selectively enhanced, and a temperature drop at the lower end of the reaction tube can be prevented.
- the lower end side coil is a coil whose radio frequency power is controlled independently of the coil above it.
- the lower end coil is divided from the coil above it, and for example, the power to supply high frequency power to the lower end coil with a power source different from the upper coil, or tap using the same power source as the upper coil
- the power to supply high frequency power to the lower end coil with a power source different from the upper coil, or tap using the same power source as the upper coil
- a heat retaining member for suppressing heat radiation from the reaction tube may be provided on the outer peripheral side of the reaction tube.
- the lower end of the reaction tube depends on its shape and the like, but, for example, from the intersection of the horizontal plane contacting the lowermost end of the reaction tube and the central axis of the reaction tube, A straight line in the direction in which the formed angle is 45 degrees,
- the upper limit is an intersection point between a shortest straight line of the straight line that equally divides the opening shape of the reaction tube into two and a perpendicular that is directed in the axial direction along the inner peripheral surface of the reaction tube.
- the silicon production apparatus of the present invention when the inner surface of the reaction tube is set to a temperature equal to or higher than the melting point of silicon and the precipitated silicon is dropped to the lower collecting portion and collected, the temperature at the lower end of the reaction tube is reduced. It is possible to prevent the solidification of the molten silicon at the lower end due to the decrease.
- FIG. 1 is a sectional view showing an embodiment of the silicon manufacturing apparatus of the present invention. Note that the conventional silicon The parts corresponding to the members and the like of the manufacturing equipment are abbreviated with reference numeral 100.
- the silicon manufacturing apparatus 1 includes a reaction vessel 2, a gas supply port 3 for supplying chlorosilanes and hydrogen, and a high-frequency heating coil provided on the outer periphery of the reaction pipe 2 in a closed vessel 11. 4 and a carbon tube 21 provided near the outer peripheral surface of the reaction tube 2 from the upper side to the vicinity of the lower end 2a.
- chlorosilanes used in the reaction include, for example, trichlorosilane (SiHCl, tetrachlorosilane (SiCl), dichlorosilane (SiH C1), monochlorosilane (SiH C1), or hexachlorodisilane (Si C1). And chlorotrisilanes such as octachlorotrisilane (SiC1), etc. These chlorosilanes may be used alone or in combination of two or more. Good.
- the reaction tube 2 is formed in a cylindrical shape such as a cylindrical shape, and is opened downward from the opening of the lower end 2a.
- a carbon material such as graphite, which can be heated by high frequency and has a resistance at the melting point of silicon, is preferably used.
- Chlorosilanes and hydrogen are supplied to the inside of the reaction tube 2 simultaneously or separately from the gas supply port 3 of the gas supply tube 6 installed above the reaction tube 2.
- the gas supply pipe 6 is preferably provided with a cooling means for cooling the gas supply pipe 6 in order to prevent thermal deterioration of the pipe and prevent decomposition of chlorosilanes in the pipe.
- the gas supply pipe 6 is cooled by, for example, providing a flow path for supplying a refrigerant liquid such as water or heat transfer oil in the gas supply pipe 6 to cool the gas supply pipe 6.
- These nozzles are installed approximately concentrically to supply the reaction gas from the gas supply pipe 6 and supply (purge) the cooling gas to the gap between the gas supply pipe 6 and each nozzle on the outer periphery of the nozzle to cool the gas.
- the cooling is performed by an air-cooled jacket system in which the gas supply pipe 6 is cooled.
- a region where the inner surface of the reaction tube 2 and the outer surface of the gas supply tube 6 overlap in the lateral direction in the upper part of the reaction tube 2 is a low temperature region, and the deposited solid silicon is heated to a melting point or higher. Since it is difficult to melt, hydrogen gas and aluminum gas are filled in the gap 7 between the reaction tube 2 and the gas supply tube 6. Gap gas or the like is supplied to fill the gap 7 with a seal gas atmosphere, thereby preventing a mixed gas of chlorosilanes and hydrogen from entering the gap 7.
- a reactant such as hydrogen chloride which reacts with silicon to generate a raw material gas may be supplied to the gap 7 alone or together with the seal gas.
- a sealing gas or the like is similarly supplied to fill the region. I have.
- the reaction tube 2 is heated by electromagnetic waves (high frequency) from the high-frequency heating coil 4 on the outer periphery, and the inner surface of the reaction tube 2 can be heated to a temperature higher than or equal to the melting point of silicon, or silicon can be deposited therebelow. Heated to a suitable temperature.
- This heating region is usually a region extending from the lower end 2a in the tube direction and having a length of 30 90% of the total length of the reaction tube 2 in the closed vessel 11.
- the inner surface of the reaction tube 2 is set to a temperature equal to or higher than the melting point of silicon (approximately 1410 to 1430 ° C). Silicon is deposited in a molten state.
- the temperature of the inner surface of the reaction tube 2 is set to, for example, 950 ° C. or higher, preferably 1200 ° C.
- the silicon is deposited at a temperature of at least C, more preferably at least 1300 ° C.
- the high-frequency heating coil 4 generates an electromagnetic wave when the coil 4 is energized from a power supply (not shown) to heat the reaction tube 2.
- the frequency of this electromagnetic wave is set to an appropriate value in accordance with the material or shape of the reaction tube 2 or the like to be heated, for example, from several tens Hz to several tens GHz.
- the silicon deposited on the inner surface of the reaction tube 2 is dropped from the opening of the lower end 2a of the reaction tube 2 and collected by the silicon recovery unit 5 provided in the falling direction.
- Metal, ceramics, glass, etc. can be used as a material for forming the cooling recovery chamber in the silicon recovery section 5.
- a metal The inner surface of the cooling and recovery chamber is preferably lined with silicon, Teflon (registered trademark), quartz glass, tantalum, tungsten, molybdenum, or the like. Silicon particles may be spread on the bottom of the cooling and recovery chamber.
- the solidified solid from the cooling and recovery chamber An outlet for continuously or intermittently extracting the recon may be provided.
- the silicon that has reached the cooling and recovery chamber is cooled by installing a force S for cooling by contact with the above materials, a cooling jacket through which the coolant liquid flows, and a cooling gas supply pipe through which the cooling gas is supplied. May be used.
- the silicon melt precipitated in a molten state is continuously dropped from the opening of the lower end 2 a of the reaction tube 2, and is recovered by the silicon recovery unit 5 installed in the falling direction. I do.
- the precipitated silicon melt flows downward along the inner surface of the reaction tube 2, falls naturally from the lower end 2 a as droplets, and solidifies during or after dropping.
- silicon is once deposited as a solid on the inner surface of the reaction tube 2, and then the inner surface is heated and heated until the temperature becomes equal to or higher than the melting point of silicon.
- silicon is deposited on the inner surface of the reaction tube 2 and the silicon is deposited on the inner surface of the reaction tube 2 until the inner surface becomes higher than the melting point of silicon.
- the steps of heating, raising the temperature, dropping the precipitate, and collecting the precipitate in the silicon collecting section 5 are repeated.
- the plate-like body is slid laterally between the space above the apparatus including the reaction tube 2 and the recovery unit 5 therebelow.
- the silicon 9 recovered in the recovery unit 5 can be taken out of the apparatus while maintaining the reaction gas atmosphere in the space above the apparatus and continuing the precipitation reaction.
- the heating for raising the inner surface of the reaction tube 2 to the melting point of silicon or more is performed by adjusting the power output of the high-frequency heating coil 4.
- the gas flowing inside the silicon manufacturing apparatus 1 is also used. This heating can be performed by reducing the flow rate of the gas.
- the conditions for producing silicon are not particularly limited, but chlorosilanes and hydrogen are mixed so that silicon is produced under conditions where the conversion of chlorosilanes to silicon is 20% or more, preferably 30% or more. It is desirable to determine the supply ratio, supply amount, stay time, etc.
- the mole fraction of chlorosilanes in the feed gas is from preferably from 0.1 99.9 mole 0/0 device Preferably it is 5 to 50 mol%. Also, higher reaction pressure has the advantage that the device can be downsized. , 0—IMPaG is easy to implement industrially.
- the residence time of the gas varies depending on the conditions of pressure and temperature for a reaction vessel of a fixed volume, but under the reaction conditions, the average residence time of the gas in the reaction tube 2 is 0.00160 seconds, If it is preferably set to 0.0110 seconds, it is possible to obtain a sufficiently economical conversion rate of chlorosilanes.
- the reaction tube 2 When the inner surface of the reaction tube 2 is set to a temperature equal to or higher than the melting point of silicon and silicon is dropped from the lower end 2a of the reaction tube 2 and collected by the silicon recovery unit 5, the reaction tube 2 is heated by the high-frequency heating coil 4.
- the lower end portion 2a is not able to sufficiently raise the temperature due to particularly large heat radiation, and the temperature is lower than that of the pipe inner surface above the lower end portion 2a. Therefore, the molten silicon is cooled at the lower end 2a, and a part thereof is solidified.
- the silicon lump is formed to extend downward from the tip of the lower end 2a in an icicle-like manner, which hinders recovery by an appropriate drop to the silicon recovery section 5. Will be done.
- a temperature lowering preventing means for preventing a lowering of the temperature of the lower end portion 2a is provided.
- the means for preventing the temperature from decreasing is, specifically, an apparatus for heating the lower end 2a of the reaction tube 2 so that the lower end 2a has a temperature equal to or higher than the melting point of silicon, preferably 1430 ° C. to 1500 ° C. , Members and the like. Excessive heating of the lower end portion 2a by the temperature lowering preventing means is not preferable because silicon fine powder is generated.
- the range of the lower end 2a to be heated by the temperature lowering prevention means depends on the shape and the like, but is as follows. That is, as shown in FIG. 9 (a), the angle between the horizontal surface (opening surface) 71 contacting the lowermost end of the reaction tube 2 and the central axis of the reaction tube 2 and the opening surface 71 is 45 degrees. Of the reaction tube 2 from the shortest straight line (for example, if the opening surface 71 has an elliptical shape) on the straight line heading in the direction Direction force in the axial direction along the inner peripheral surface Range force up to the horizontal plane 72 passing through the intersection 74 with the vertical line The lower end 2a to be heated by the above-mentioned temperature reduction prevention means.
- the opening shape of the reaction tube 2 may be other shapes such as an elliptical shape in addition to a circular shape.
- This opening The shape of the lower end portion 2a in the vicinity of the mouth is not limited to the case where the thickness of the silicon melt is adjusted so that the silicon particle diameter is small and uniform, in addition to the case where the thickness is uniform from above to the lowermost end.
- the outer peripheral portion may be cut obliquely so that the diameter of the outer peripheral portion gradually decreases toward the lower end, or the opening may have a wavy shape.
- the opening surface of the reaction tube 2 may be slightly inclined from a horizontal plane.
- the range of the lower end 2a to be heated by the above-mentioned temperature drop prevention means is defined by the intersection 73 between the opening surface 71 of the reaction tube 2 and the central axis of the reaction tube 2.
- the range where the distance from these intersections 74a and 74b is equal and the upper limit is the parallel surface 72 parallel to the opening surface 71 is heated by the above-mentioned temperature drop prevention means.
- the lower end 2a should be.
- the range of heating by the above-mentioned temperature reduction prevention means is a region of the lower end portion 2a (the lowermost force of the reaction tube 2 is also a length range up to the distance r in the tube axis direction). It is indispensable, and if necessary, it is desirable to heat the length range (4r) up to four times this distance r by the above-mentioned temperature drop prevention means.
- silicon fine powder may be generated.
- D is 2 or more, preferably 3 or more.
- the heat retaining member 23 is not necessarily required and may be kept warm.
- the member 23 may be omitted. Even when the lower end 2a of the reaction tube 2 is covered to the lowermost end by the heat retaining member 23, the temperature of the lower end 2a decreases due to heat radiation from the inner surface of the lower end 2a, and the heat retaining member 23 When the lower end 2a is not covered, the temperature drop of the lower end 2a is larger.
- the lower end 2a is A carbon tube 21 is provided to cover the outer periphery in the vicinity.
- the carbon tube 21 is formed using a carbon material, such as graphite, which can be heated by high frequency from the high frequency heating coil 4 as a base material.
- the lower end 2a of the reaction tube 2 is directly heated by the high-frequency heating coil 4 and simultaneously heated by infrared rays emitted from the carbon tube 21 heated by the high-frequency heating coil 4.
- the lower end 2a is sufficiently heated and heated to a temperature equal to or higher than the melting point of silicon.
- the molten silicon which does not form a lump, falls along the inner surface of the reaction tube 2 and smoothly falls from the lower end 2a, and is collected by the silicon collecting unit 5.
- the carbon tube 21 is installed so as to separate the reaction tube 2 from a heat insulating member 23 formed of a carpon fiber, a ceramic sintered body, or the like provided on the outer periphery of the reaction tube 2.
- a heat insulating member 23 is wound around the heat insulating member.
- a sealing gas such as hydrogen is supplied to a gap 24 between the reaction tube 2 and the carbon tube 21 to prevent silicon deposition in this region.
- a tubular member separating the reaction tube 2 and the heat retaining member 23 as in the carbon tube 21 of FIG. 1 a part including a lower end thereof is formed of a carbon material, and an upper portion thereof is formed of a ceramic or the like.
- a coil formed of a material that is not heated by the high frequency from the high frequency heating coil 4 may be used. That is, if the tubular member is formed of a carbon material near the lower end 2a of the reaction tube 2, infrared heating can be performed on the lower end 2a, and other portions of the tubular member are made of a material other than the carbon material. It is formed of
- a heat retaining member 23 may be wound around the outer surface of the reaction tube 2, and the carbon tube 21 may be installed only near the lower end 2a of the reaction tube 2.
- the thickness of the carbon tube 21 in the radial direction is determined in consideration of the penetration depth by the frequency and the strength, etc., in order for the high frequency from the high frequency heating coil 4 to efficiently reach the lower end 2a of the reaction tube 2. It is desirable that the thickness be as thin as possible.
- FIGS. 3 and 4 are cross-sectional views showing the vicinity of the lower end of the reaction tube in another embodiment of the silicon manufacturing apparatus of the present invention.
- a ring-shaped heating element 31 is arranged near the lower end 2a of the reaction tube 2, and a current is supplied to the ring-shaped heating element 31 from a power supply (not shown) to heat and heat the ring-shaped heating element 31.
- a power supply not shown
- Infrared from ring-shaped heating element 31 to lower end 2a The lower end 2a is heated by irradiating a line.
- a plurality of rods 41 made of quartz glass are arranged near the lower end 2 a of the reaction tube 2, and infrared light from the light bulb 42 is transmitted to the base 4 of the rod 41.
- the light is introduced from la into the inside of the rod-shaped body 41 and guided to the tip 41b.
- the lower end 2a is heated by spot irradiation of infrared light from the front end 41b to the lower end 2a.
- the tip portion 41b of the rod-shaped body 41 made of quartz glass is desirably formed in a lens shape in order to converge emitted infrared light.
- the lower end 2a of the reaction tube 2 is heated by infrared rays to prevent the temperature from lowering.
- the infrared rays are irradiated over the entire circumference of the lower end 2a to be heated. It is desirable.
- FIG. 5 is a cross-sectional view showing the vicinity of the lower end of a reaction tube in another embodiment of the silicon manufacturing apparatus of the present invention.
- the high-frequency heating coil 4 is formed with a coil pitch P1 shorter than the coil pitch P2 of the coil 4U above the coil in the region near the lower end 2a of the reaction tube 2 (lower end coil 4L) t. (See Figure 1 for the overall layout of the lower coil 4L and coil 4U).
- a single power supply As a power supply for supplying power to the high-frequency heating coil 4, a single power supply is provided.
- the lower coil 2L emits a high frequency higher than the high frequency from the coil 4U above the lower coil 4L, and the lower end 2a of the reaction tube 2 is selectively and strongly heated.
- the lower end portion 2a of the reaction tube 2 and the upper portion thereof can be heated by the same power supply, so that a relatively simple device configuration can be achieved.
- FIG. 6 is a sectional view showing a modification of the embodiment of FIG.
- a carbon tube 21 is provided near the lower end 2 a of the reaction tube 2.
- the carbon tube 21 is heated by the lower end coil 4L having a high winding density, and the lower end 2a of the reaction tube 2 is heated by infrared rays radiated from the heated carbon tube 21.
- the lower end 2a of the reaction tube 2 is selectively and strongly heated by the lower end coil 4L having a high winding density, and further heated by infrared rays from the carbon tube 21 heated by the high frequency from the lower end coil 4L. Therefore, it is possible to effectively prevent a temperature drop at the lower end 2a of the reaction tube 2.
- FIG. 7 is a cross-sectional view showing the vicinity of the lower end of the reaction tube in another embodiment of the silicon manufacturing apparatus of the present invention.
- the coil (lower end coil 4L) of the high-frequency heating coil 4 in the region near the lower end 2a of the reaction tube 2 is formed of two coils that are wound twice in the diameter increasing direction.
- the lower end coil 4L is wound twice as described above, when the reaction tube 2 is heated by the high-frequency heating coil 4, the lower end 2a of the reaction tube 2 becomes the inner coil and the outer coil of the lower end coil 4L. It is heated by the high frequency waves from both of them, and is heated more strongly than the heating from the coil 4U above it. Therefore, the lower end 2a of the reaction tube 2 is selectively and strongly heated, and a temperature drop at the lower end 2a is prevented.
- the lower end coil 4L may be a double wound coil or a multiple wound coil wound three or more times in the diameter expanding direction.
- a single power supply can be used when the lower end coil 4L is formed by winding one coil in a multiplex manner.
- FIG. 8 is a cross-sectional view showing the vicinity of the lower end of the reaction tube in another embodiment of the silicon manufacturing apparatus of the present invention.
- the high-frequency heating coil 4 is composed of two divided coils to which power is supplied by different systems.
- One coil 4U is installed on the outer peripheral side of the entire deposition region above the vicinity of the lower end 2a of the reaction tube 2, and the other lower end coil 4L is installed in the vicinity of the lower end 2a of the reaction tube 2.
- These coils 4U and 4L at the lower end have a high frequency by an independent control system of another system.
- the wave power is controlled, the deposition region above the lower end 2a of the reaction tube 2 is heated by the coil 4U, and the lower end 2a is heated by the coil 4L.
- each control system When melting the silicon, each control system is set so that the heating intensity of the lower end coil 4L to the lower end 2a of the reaction tube 2 is higher than the heating intensity of the upper coil 4L to the reaction tube 2.
- To control the high frequency power Thereby, the lower end 2a of the reaction tube 2 is selectively and strongly heated by the strong high frequency generated by the lower end coil 4L, and the lowering of the temperature at the lower end 2a is prevented.
- a power supply for supplying power to the coil 4U and a power supply for supplying power to the lower coil 4L are provided.
- a method of supplying high frequency power to each coil independently from each power source there is a method of supplying high frequency power to each coil independently from each power source.
- the power supply for supplying power to the coil 4U and the power supply for supplying power to the lower coil 4L are the same power supply, and the power supply system is made independent by taps, thyristors, etc., and high-frequency power is supplied to these coils by separate systems. You may make it supply.
- the supply of the high-frequency power to the lower end coil 4L is adjusted by measuring the temperature of the lower end 2a of the reaction tube 2 and visually confirming the feedback control force or the operating state.
- a reaction tube having a carbon material, dimensions of 100 mm in outer diameter, 70 mm in inner diameter, and 1000 mm in length was attached to a polycrystalline silicon manufacturing apparatus.
- a carbon tube (21) is installed on the outer peripheral side of the lower end of the reaction tube as shown in Fig. 2, and the lower end of the reaction tube is heated by infrared rays from the carbon tube heated by the high-frequency heating coil. I made it.
- a mixed gas of 20 kg / H of trichlorosilane and 40 Nm 3 / H of hydrogen is passed through the inside of the reaction tube, and heated by a high-frequency heating coil wound at a uniform coil pitch, so that the temperature at the bottom and bottom of the reaction tube was raised to 1450 ° C. or higher to deposit polycrystalline silicon in a molten state. After the continuous reaction for 100 hours, the state of the lower end of the reaction tube was observed, but the silicon lump was not solidified at the lower end of the reaction tube.
- a reaction tube having a carbon material, dimensions of 100 mm in outer diameter, 70 mm in inner diameter, and 1000 mm in length was attached to a polycrystalline silicon manufacturing apparatus.
- the high-frequency heating coil of this silicon manufacturing apparatus used a lower-end coil (a coil having a shorter pitch of 4U and a higher winding density.
- the pitch P1 of the lower-end coil (4L) was used.
- High-frequency power was supplied from the same power supply to these successively wound coils with a pitch P2 of 10 mm and a pitch P2 of the upper coil (4U) of 30 mm.
- a mixed gas of 20 kg / H of trichlorosilane and 40 Nm 3 / H of hydrogen is passed through the inside of the reaction tube, and heated by the high-frequency heating coil to a temperature of 1450 ° C at the lower end of the reaction tube and at a temperature other than the lower end.
- the temperature was raised as described above, and polycrystalline silicon was precipitated in a molten state. After the continuous reaction for 100 hours, the state of the lower end of the reaction tube was observed. At the lower end of the reaction tube, no silicon lump was solidified.
- a reaction tube having a carbon material, dimensions of 100 mm in outer diameter, 70 mm in inner diameter, and 1000 mm in length was attached to a polycrystalline silicon manufacturing apparatus.
- the high-frequency heating coil of the silicon manufacturing apparatus used was a coil in which the lower end side coil (4L) was wound twice in the diameter increasing direction.
- a mixed gas of 20 kg / H of trichlorosilane and 40 Nm 3 / H of hydrogen is passed through the inside of the reaction tube, and heated by the high-frequency heating coil to raise the temperature at the lower end of the reaction tube and at a temperature other than the lower end to 1450 ° C.
- the temperature was raised as described above, and polycrystalline silicon was precipitated in a molten state. After the continuous reaction for 100 hours, the state of the lower end of the reaction tube was observed. At the lower end of the reaction tube, no silicon lump was solidified.
- a reaction tube having a carbon material, dimensions of 100 mm in outer diameter, 70 mm in inner diameter, and 1000 mm in length was attached to a polycrystalline silicon manufacturing apparatus.
- the high-frequency heating coil of this silicon manufacturing equipment separates the high-frequency power to the lower coil (4L) and the high-frequency power to the upper coil (4U) in separate systems.
- the power supply for the lower coil (4L) and the power supply for the coil The power supply to each of these divided coils is independently controlled.
- a mixed gas of 20 kg / H of trichlorosilane and 40 Nm 3 / H of hydrogen is passed through the inside of the reaction tube, and heated by the high-frequency heating coil to raise the temperature at the lower end of the reaction tube and at a temperature other than the lower end to 1450 ° C.
- the temperature was raised as described above, and polycrystalline silicon was precipitated in a molten state. After the continuous reaction for 100 hours, the state of the lower end of the reaction tube was observed. At the lower end of the reaction tube, no silicon lump was solidified.
- a continuous reaction was carried out under the same conditions as in Example 1 except that the carbon tube (21) was not provided, but a silicon lump solidified at the lower end of the reaction tube and formed an icicle-like extension. This silicon lump made it impossible to continue the reaction.
- FIG. 1 is a cross-sectional view showing an embodiment of a silicon manufacturing apparatus of the present invention.
- FIG. 2 is a cross-sectional view of the vicinity of the lower end of a reaction tube, showing a modification of the embodiment of FIG. 1.
- FIG. 3 is a cross-sectional view showing a periphery of a lower end portion of a reaction tube in another embodiment of the silicon manufacturing apparatus of the present invention.
- FIG. 4 is a cross-sectional view showing a periphery of a lower end portion of a reaction tube in another embodiment of the silicon manufacturing apparatus of the present invention.
- FIG. 5 is a cross-sectional view showing the periphery of the lower end of a reaction tube in another embodiment of the silicon manufacturing apparatus of the present invention.
- FIG. 6 is a cross-sectional view of the vicinity of a lower end portion of a reaction tube showing a modification of the embodiment of FIG. 5.
- FIG. 7 is a cross-sectional view showing a periphery of a lower end portion of a reaction tube in another embodiment of the silicon manufacturing apparatus of the present invention.
- FIG. 8 is a cross-sectional view showing the periphery of the lower end of a reaction tube in another embodiment of the silicon manufacturing apparatus of the present invention.
- Fig. 9 is a diagram for explaining the range of the lower end of the reaction tube to be heated by the temperature lowering prevention means.
- FIG. 10 is a diagram illustrating a range of heating by a temperature drop prevention unit.
- FIG. 11 shows the length L of the silicon deposition portion of the reaction tube and the reaction tube in the apparatus of the present invention.
- Fig. 9 is a diagram for explaining a ratio L / D to an inner diameter D at the lowermost end of the graph c.
- FIG. 12 is a cross-sectional view showing a conventional manufacturing apparatus. Explanation of symbols
Abstract
Description
Claims
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US10/569,149 US7993455B2 (en) | 2003-08-22 | 2004-08-17 | Silicon manufacturing apparatus |
AU2004266934A AU2004266934B2 (en) | 2003-08-22 | 2004-08-17 | Silicon manufacturing apparatus |
EP04771735A EP1666414A4 (en) | 2003-08-22 | 2004-08-17 | DEVICE FOR PRODUCING SILICON |
CA002517764A CA2517764C (en) | 2003-08-22 | 2004-08-17 | Silicon production apparatus |
JP2005513280A JP4597863B2 (ja) | 2003-08-22 | 2004-08-17 | シリコン製造装置 |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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JP2003-298641 | 2003-08-22 | ||
JP2003298641 | 2003-08-22 |
Publications (1)
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WO2005019106A1 true WO2005019106A1 (ja) | 2005-03-03 |
Family
ID=34213722
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Application Number | Title | Priority Date | Filing Date |
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PCT/JP2004/011774 WO2005019106A1 (ja) | 2003-08-22 | 2004-08-17 | シリコン製造装置 |
Country Status (7)
Country | Link |
---|---|
US (1) | US7993455B2 (ja) |
EP (1) | EP1666414A4 (ja) |
JP (1) | JP4597863B2 (ja) |
CN (1) | CN100347083C (ja) |
AU (1) | AU2004266934B2 (ja) |
CA (1) | CA2517764C (ja) |
WO (1) | WO2005019106A1 (ja) |
Cited By (3)
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WO2011061847A1 (ja) * | 2009-11-20 | 2011-05-26 | Kaneko Kyojiro | シリコン電磁鋳造装置 |
RU2550863C2 (ru) * | 2009-12-25 | 2015-05-20 | Консарк Корпорейшн | Установка для электромагнитного литья кремния |
AU2013204598B2 (en) * | 2009-11-20 | 2015-12-24 | Consarc Corporation | Electromagnetic casting apparatus for silicon |
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US7727483B2 (en) * | 2004-08-19 | 2010-06-01 | Tokuyama Corporation | Reactor for chlorosilane compound |
KR100768147B1 (ko) * | 2006-05-11 | 2007-10-18 | 한국화학연구원 | 혼합된 코어수단을 이용한 다결정 실리콘 봉의 제조방법과그 제조장치 |
WO2009084627A1 (ja) * | 2007-12-28 | 2009-07-09 | Tokuyama Corporation | シリコン製造装置 |
RU2388690C2 (ru) * | 2008-05-22 | 2010-05-10 | Общество с ограниченной ответственностью "Группа СТР" | Способ получения поликристаллического кремния |
US20110070370A1 (en) * | 2008-05-28 | 2011-03-24 | Aixtron Ag | Thermal gradient enhanced chemical vapour deposition (tge-cvd) |
JP5334490B2 (ja) * | 2008-08-06 | 2013-11-06 | 株式会社トクヤマ | シリコン製造装置 |
CN103787336B (zh) | 2008-09-16 | 2016-09-14 | 储晞 | 生产高纯颗粒硅的方法 |
NO334785B1 (no) | 2009-05-29 | 2014-05-26 | Dynatec Engineering As | Reaktor og fremgangsmåte for fremstilling av silisium |
KR101708058B1 (ko) * | 2009-07-15 | 2017-02-17 | 미쓰비시 마테리알 가부시키가이샤 | 다결정 실리콘의 제조 방법, 다결정 실리콘의 제조 장치, 및 다결정 실리콘 |
JP5655429B2 (ja) | 2009-08-28 | 2015-01-21 | 三菱マテリアル株式会社 | 多結晶シリコンの製造方法、製造装置及び多結晶シリコン |
US20110097495A1 (en) * | 2009-09-03 | 2011-04-28 | Universal Display Corporation | Organic vapor jet printing with chiller plate |
JP5500953B2 (ja) * | 2009-11-19 | 2014-05-21 | 株式会社ニューフレアテクノロジー | 成膜装置および成膜方法 |
KR101329030B1 (ko) * | 2010-10-01 | 2013-11-13 | 주식회사 실리콘밸류 | 유동층 반응기 |
KR101356391B1 (ko) * | 2011-04-20 | 2014-02-03 | 주식회사 실리콘밸류 | 다결정 실리콘 제조장치 |
TWI506261B (zh) * | 2014-01-27 | 2015-11-01 | Vacuum desorption device after sample gas concentration | |
KR101821006B1 (ko) | 2014-05-13 | 2018-01-22 | 주식회사 엘지화학 | 수평형 반응기를 이용한 폴리실리콘 제조 장치 및 제조 방법 |
WO2018051304A1 (en) | 2016-09-19 | 2018-03-22 | King Abdullah University Of Science And Technology | Susceptor |
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- 2004-08-17 EP EP04771735A patent/EP1666414A4/en not_active Withdrawn
- 2004-08-17 US US10/569,149 patent/US7993455B2/en not_active Expired - Fee Related
- 2004-08-17 JP JP2005513280A patent/JP4597863B2/ja not_active Expired - Fee Related
- 2004-08-17 AU AU2004266934A patent/AU2004266934B2/en not_active Ceased
- 2004-08-17 CN CNB2004800093439A patent/CN100347083C/zh not_active Expired - Fee Related
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Also Published As
Publication number | Publication date |
---|---|
CN100347083C (zh) | 2007-11-07 |
US20070034146A1 (en) | 2007-02-15 |
CA2517764C (en) | 2009-10-13 |
CA2517764A1 (en) | 2005-03-03 |
AU2004266934B2 (en) | 2010-03-11 |
EP1666414A4 (en) | 2009-07-15 |
AU2004266934A1 (en) | 2005-03-03 |
US7993455B2 (en) | 2011-08-09 |
CN1771195A (zh) | 2006-05-10 |
JP4597863B2 (ja) | 2010-12-15 |
EP1666414A1 (en) | 2006-06-07 |
JPWO2005019106A1 (ja) | 2006-10-19 |
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