KR101057101B1 - Fluidized bed reactor for producing granular polycrystalline silicon and method of producing the same - Google Patents

Fluidized bed reactor for producing granular polycrystalline silicon and method of producing the same Download PDF

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Publication number
KR101057101B1
KR101057101B1 KR1020100099457A KR20100099457A KR101057101B1 KR 101057101 B1 KR101057101 B1 KR 101057101B1 KR 1020100099457 A KR1020100099457 A KR 1020100099457A KR 20100099457 A KR20100099457 A KR 20100099457A KR 101057101 B1 KR101057101 B1 KR 101057101B1
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chamber
silicon
fluidized bed
bed reactor
producing
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KR1020100099457A
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Korean (ko)
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임천수
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(주)기술과가치
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Priority to PCT/KR2011/007522 priority patent/WO2012050341A2/en

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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
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/1818—Feeding of the fluidising gas
    • B01J8/1827—Feeding of the fluidising gas the fluidising gas being a reactant
    • 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
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/24—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique
    • B01J8/38—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique with fluidised bed containing a rotatable device or being subject to rotation or to a circulatory movement, i.e. leaving a vessel and subsequently re-entering it
    • B01J8/384—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique with fluidised bed containing a rotatable device or being subject to rotation or to a circulatory movement, i.e. leaving a vessel and subsequently re-entering it being subject to a circulatory movement only
    • B01J8/386—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique with fluidised bed containing a rotatable device or being subject to rotation or to a circulatory movement, i.e. leaving a vessel and subsequently re-entering it being subject to a circulatory movement only internally, i.e. the particles rotate within the vessel
    • 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
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008—Controlling the process
    • B01J2208/00017—Controlling the temperature
    • B01J2208/00106—Controlling the temperature by indirect heat exchange
    • B01J2208/00115—Controlling the temperature by indirect heat exchange with heat exchange elements inside the bed of solid particles
    • B01J2208/00132—Tubes
    • 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
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008—Controlling the process
    • B01J2208/00017—Controlling the temperature
    • B01J2208/00106—Controlling the temperature by indirect heat exchange
    • B01J2208/00115—Controlling the temperature by indirect heat exchange with heat exchange elements inside the bed of solid particles
    • B01J2208/0015—Plates; Cylinders
    • 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
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008—Controlling the process
    • B01J2208/00017—Controlling the temperature
    • B01J2208/00477—Controlling the temperature by thermal insulation means
    • B01J2208/00495—Controlling the temperature by thermal insulation means using insulating materials or refractories
    • 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
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00796—Details of the reactor or of the particulate material
    • B01J2208/00893—Feeding means for the reactants
    • B01J2208/00902—Nozzle-type feeding elements
    • 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
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00796—Details of the reactor or of the particulate material
    • B01J2208/00991—Disengagement zone in fluidised-bed reactors
    • 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
    • B01J2219/025—Apparatus characterised by their chemically-resistant properties characterised by the construction materials of the reactor vessel proper
    • B01J2219/0277—Metal based
    • B01J2219/0286—Steel

Abstract

The present invention relates to a fluidized bed reactor for producing particulate polysilicon and a method for producing polycrystalline silicon using the same. More particularly, in a fluidized bed reactor for producing particulate polycrystalline silicon in which a reaction is performed at the top of the chamber by injecting a fluid gas from the bottom of the chamber. chamber; A tubular heating device located inside the chamber; A flow gas first supply pipe formed under the chamber to supply the flow gas into the heating device; And it provides a fluidized bed reactor for producing a particulate polycrystalline silicon and a polycrystalline silicon manufacturing method using the same, characterized in that it comprises a venturi to increase the flow gas velocity inside the heating device.

Description

Fluidized bed reactor for producing granular polycrystalline silicon and method for producing polycrystalline silicon using same {Fluidized Bed Reactor for Producing Granular Polycrystalline Silicon and Method of Producing the Same}

The present invention relates to a fluidized bed reactor for producing polycrystalline silicon and a method for producing polycrystalline silicon using the same, and more particularly, in the production of a large amount of polycrystalline silicon in the form of particles using a fluidized bed reactor, silicon is deposited in a heating apparatus. The present invention relates to a fluidized bed reactor for producing polycrystalline silicon and a method for producing polycrystalline silicon using the same, which efficiently prevents accumulation and not only continuously operate the reactor but also select particle sizes and produce high purity silicon particles.

In order to prepare polycrystalline silicon, a chemical vapor deposition (CVD) method in which a silicon component is continuously deposited on a surface of a seed particle silicon by pyrolysis or hydrogen reduction of a reaction gas containing a silicon component is generally used. However, this process is a batch process with a long production time.

As such, a bell jar type reactor has been mainly used for commercial mass production of polycrystalline silicon used in the semiconductor field, and the diameter of the polycrystalline silicon product manufactured using the reactor is about 50 to 300 mm. . Since the vertical reactor, in which electric resistance heating is the core, has a limit on the diameter of the rod that increases due to the precipitation of silicon, not only the product cannot be continuously produced, but also the power consumption for maintaining the surface of the silicon rod at a reaction temperature of about 1,000 ° C. or more is very large. It has a disadvantage. Due to this limitation, the process is forced to proceed to a batch process.

Therefore, in order to solve this disadvantage, recently, a silicon precipitation process using a fluidized bed reactor capable of continuously producing polycrystalline silicon in the form of particles having a size of about 0.5 to 3.0 mm has been developed. According to this method, the silicon particles form a fluidized bed by the flowing gas supplied from the lower part of the reactor to the upper direction, and the silicon component in the reaction gas is bonded to the surface of these silicon particles heated to a high temperature so that the particles grow. To produce polycrystalline silicon products. At this time, the small size silicon seed particles (種 粒子, seed crystal) is lost to the fluidity as it increases due to the continuous precipitation of the silicon component gradually sinks to the bottom of the fluidized bed. The product particles thus grown are sorted and discharged toward the product collection, while ungrown particles are continuously introduced into the fluidized bed and continue to precipitate. Here, the silicon seed particles can be continuously or periodically filled into the fluidized bed.

Polycrystalline silicon prepared using a fluidized bed reactor as described above is mainly used for the production of silicon single crystal, which is a basic material of semiconductor wafers. In addition, the fluidized bed reactor has a very large surface area of the silicon particles that can be precipitated, the reaction yield is high under the same reaction conditions, there is an advantage that the reaction can be maintained continuously.

However, the silicon-containing gas decomposes itself at temperatures above about 300 to 400 ° C. (initial decomposition temperature) to cause homogeneous necleation reactions, as well as on the surface of the inner wall of the fluidized bed reactor where the reaction temperature is higher than the initial decomposition temperature. Silicon precipitates regardless of the type of material. Therefore, not only silicon precipitation occurs on the surface of the flowing silicon particles, but also a phenomenon in which silicon particles accumulate in a heating apparatus or the like inside the reactor.

Accumulation of the inner wall of the reactor of the silicon precipitates not only lowers the yield of the product, but also stops the continuous operation of the fluidized bed reactor due to generation of particles or chunks out of specification. Accumulation of silicon precipitates inside the reactor not only causes breakage or degradation of the reactor and operational safety problems, but also causes physical or thermal deformation and stress caused by the layer or mass of the precipitate, causing cracks or breakage in the reactor. This can increase the risk of an accident.

Republic of Korea Patent No. 0411180 "Method and apparatus for producing polycrystalline silicon" in the production of a large amount of polycrystalline silicon in the form of a particle using a fluidized bed reactor by mounting a nozzle for supplying an etching gas containing hydrogen chloride There is disclosed a method and apparatus for producing polycrystalline silicon which effectively prevents the deposition and accumulation of silicon on the surface of the supply means and allows the reactor to be operated continuously. However, the patent discloses that the precipitated silicon particles directly contact the heating means. While falling down, there is a problem that silicon particles accumulate in the heating means. The etching process using hydrogen chloride may corrode polycrystalline silicon as a product to sacrifice yield.

In addition, US Pat. No. 7029632 discloses a radiant heat source in which a heating device is located outside the inner reaction tube and at the same time disposed around the heating zone without directly contacting the reaction tube. The radiation source reacts the silicon particles in the heating zone by radiant heat. It is characterized by heating above the temperature by radiant heat. However, the patent has a problem that the silicon particles heated by the heating device reacts and the silicon accumulates in the inner reaction tube in contact with the heating device.

In the case where the accumulation of the silicon particles occurs, the productivity is lowered by stopping the continuous process and removing the accumulated part. In addition, the fluidized bed reactor known to date has a disadvantage that the size distribution of the particles is wide because there is no method for selecting the product particles in a uniform size.

Therefore, it has been desired to develop a reactor capable of producing continuous particles while at the same time producing particles having a uniform distribution while minimizing the accumulation of silicon inside the reactor during the production of polysilicon particles.

An object of the present invention to solve the above problems is to provide a method for producing polycrystalline silicon using the fluidized bed reactor that can be prevented from accumulating in the heating device, etc. in the fluidized bed reactor.

Another object of the present invention is to provide a method for producing polycrystalline silicon using a fluidized bed reactor that can produce a uniform particle size when producing the polycrystalline silicon particles through a fluidized bed reactor.

In order to achieve the above object, the present invention provides a fluidized bed reactor for producing particulate polycrystalline silicon in which a flow gas is injected from the lower part of the chamber and reaction occurs at the upper part of the chamber. A tubular heating device located inside the chamber; A flow gas first supply pipe formed under the chamber to supply the flow gas into the heating device; And it provides a fluidized bed reactor for producing a particulate polysilicon characterized in that it comprises a venturi to increase the flow gas velocity inside the heating device.

In another aspect, the present invention provides a fluidized bed reactor for producing particulate polysilicon, characterized in that it further comprises a cone leading the silicon formed of particles in the chamber to the first supply pipe.

In another aspect, the present invention provides a fluidized bed reactor for producing particulate polysilicon, characterized in that the chamber is formed in a cone shape to guide the silicon formed of particles to the first supply pipe.

In another aspect, the present invention provides a fluidized bed reactor for producing particulate polysilicon, characterized in that it comprises a reaction gas supply pipe for supplying a reaction gas containing a silicon component to the upper portion of the chamber at a position higher than the heating device.

In another aspect, the present invention provides a fluidized bed reactor for producing particulate polysilicon, characterized in that to form a second supply pipe in the lower chamber outside the heating device to supply a flow gas to the upper chamber.

In another aspect, the present invention provides a fluidized bed reactor for producing particulate polysilicon, characterized in that it further comprises a third supply pipe for supplying a flow gas to increase the speed of the material flowing through the venturi.

In another aspect, the present invention provides a fluidized bed reactor for producing particulate polysilicon, characterized in that the silicon seed particles are introduced into the fluidized bed of the upper chamber.

In addition, the reaction gas of the present invention provides a fluidized bed reactor for producing a particulate polysilicon, characterized in that the silicon component or at least one of hydrogen, argon and helium in the silicon component.

In addition, the present invention is for producing a particulate polycrystalline silicon, characterized in that at least one selected from monosilane (SiH 4 ), dichlorosilane (SiH 2 Cl 2 ), trichlorosilane (SiHCl 3 ) and tetrachloride (SiCl 4 ) as the silicon component. Provide a fluidized bed reactor.

The present invention also provides a fluidized bed reactor for producing particulate polysilicon, wherein the flow gas is selected from at least one of hydrogen, argon and helium.

In another aspect, the present invention provides a fluidized bed reactor for producing particulate polysilicon, characterized in that the material of the chamber is any one of metal, alloy and ceramic. More specifically, the chamber provides a fluidized bed reactor for producing particulate polycrystalline silicon, characterized in that any one of stainless-steel, quartz, and carbon steel.

In another aspect, the present invention provides a fluidized bed reactor for producing particulate polysilicon, characterized in that the inner wall of the chamber is coated with any one of silicon, silicon carbide (SiC), silicon nitride (Si 3 N 4 ), Si 3 O 4 .

In another aspect, the present invention provides a fluidized bed reactor for producing particulate polysilicon, characterized in that the heating device is installed perpendicular to the lower portion of the chamber, there is a space through which the silicon particles and gas can pass.

In another aspect, the present invention is the heating device is composed of a heating unit, a reflecting surface and an insulator, wherein the heating unit is located inside the tubular shape is formed so that heat can be transferred to the upper portion of the chamber through the inside of the heating apparatus Provided is a fluidized bed reactor for producing silicon.

In another aspect, the insulator is formed on the outside of the tubular shape, the material of the insulator is any one of a ceramic, a fabric made of silica fibers, silicon carbide (SiC) and silicon nitride (Si 3 N 4 ). Provided is a fluidized bed reactor for producing particulate polycrystalline silicon.

In another aspect, the present invention provides a fluidized bed reactor for producing particulate polysilicon, characterized in that the flow gas and the reaction gas introduced into the chamber is discharged through the discharge means.

In another aspect, the present invention provides a fluidized bed reactor for producing particulate polysilicon, characterized in that the silicon seed particles discharged through the discharge means is sized and re-introduced into the chamber.

In another aspect, the present invention provides a fluidized bed reactor for producing particulate polysilicon, characterized in that the discharge means is located above the chamber.

In another aspect, the present invention provides a fluidized bed reactor for producing particulate polysilicon, characterized in that the pressure in the chamber is 1 to 20bar.

The present invention also provides a hermetic chamber; A tubular heating device located inside the chamber; A flow gas first supply pipe formed under the chamber to supply the flow gas into the heating device; And in the fluidized bed reactor including a venturi for increasing the flow gas velocity inside the heater, the silicon grown by precipitation after the fluidized bed is formed in the upper part of the heater by injecting the reaction gas and the fluid gas separately, respectively, into the chamber. It provides a method for producing particulate polysilicon characterized in that the screening down and down through the first supply pipe.

In another aspect, the present invention provides a method for producing particulate polysilicon, characterized in that it further comprises a cone leading to the silicon formed of particles in the chamber to the first supply pipe.

In another aspect, the present invention provides a method for producing particulate polysilicon, characterized in that the chamber is formed in a cone shape to guide the silicon formed of particles to the first supply pipe.

In another aspect, the present invention provides a method for producing particulate polysilicon, characterized in that it comprises a reaction gas supply pipe for supplying a reaction gas containing a silicon component to the upper portion of the chamber at a position higher than the heating device.

In another aspect, the present invention provides a method for producing particulate polysilicon, characterized in that to form a second supply pipe in the lower chamber outside the heating device to supply a flow gas to the upper chamber.

In another aspect, the present invention provides a method for producing particulate polysilicon, characterized in that it further comprises a third supply pipe for supplying a flow gas to increase the speed of the material flowing through the venturi.

In another aspect, the present invention provides a method for producing particulate polysilicon, characterized in that the silicon seed particles are introduced into the fluidized bed of the upper chamber.

In another aspect, the present invention provides a method for producing particulate polysilicon, characterized in that the reaction gas is included in the silicon component or at least one of hydrogen, argon and helium in the silicon component.

In another aspect, the present invention is the production of particulate polycrystalline silicon, characterized in that at least one selected from monosilane (SiH 4 ), dichlorosilane (SiH 2 Cl 2 ), trichlorosilane (SiHCl 3 ) and tetrachloride (SiCl 4 ) as the silicon component. Provide a method.

In another aspect, the present invention provides a method for producing particulate polysilicon, characterized in that the flow gas is selected from at least one of hydrogen, argon and helium.

In another aspect, the present invention provides a method for producing particulate polysilicon, characterized in that the material of the chamber is any one of metal, alloy and ceramic. More specifically, the chamber provides a method for producing particulate polysilicon, wherein the material is any one of stainless steel, quartz, and carbon steel.

In another aspect, the present invention provides a method for producing particulate polycrystalline silicon, characterized in that the inner wall of the chamber is coated with any one of silicon, silicon carbide (SiC), silicon nitride (Si 3 N 4 ) and Si 3 O 4 .

In another aspect, the present invention provides a method for producing particulate polysilicon, characterized in that the heating device is installed vertically in the lower portion of the chamber, there is a space through which the silicon particles and gas can pass.

In addition, the present invention is the heating device is composed of a heating unit, a reflecting surface and an insulator, wherein the heating unit is located inside the tubular shape is formed so that heat can be transferred to the upper portion of the chamber through the interior of the heating apparatus It provides a silicon manufacturing method.

In another aspect, the insulator is formed on the outside of the tubular shape, the material of the insulator is any one of a ceramic, a fabric made of silica fibers, silicon carbide (SiC) and silicon nitride (Si 3 N 4 ). It provides a particulate polysilicon production method.

In another aspect, the present invention provides a method for producing particulate polysilicon, characterized in that the flow gas and the reaction gas introduced into the chamber is discharged through the discharge means.

In another aspect, the present invention provides a method for producing particulate polysilicon, characterized in that the silicon seed particles discharged through the discharge means is sized and re-introduced into the chamber.

In another aspect, the present invention provides a method for producing particulate polysilicon, characterized in that the discharge means is located above the chamber.

In another aspect, the present invention provides a method for producing particulate polysilicon, characterized in that the pressure in the chamber is 1 to 20bar.

The fluidized bed reactor for producing particulate polycrystalline silicon and the polycrystalline silicon manufacturing method using the same according to the present invention have an advantage that a phenomenon in which silicon particles accumulate in a heating apparatus is hardly generated.

In addition, the fluidized bed reactor for producing particulate polycrystalline silicon and the polycrystalline silicon manufacturing method using the same according to the present invention can be produced according to the particle size of the desired polycrystalline silicon by controlling the speed of the flow gas supplied from the first supply pipe, the second supply pipe and the third supply pipe. It has an effect.

In addition, the fluidized bed reactor for producing particulate polycrystalline silicon and the polycrystalline silicon manufacturing method using the same according to the present invention have a continuous process, and thus have an effect of long-term use and productivity.

In addition, the fluidized bed reactor for producing particulate polycrystalline silicon and the polycrystalline silicon manufacturing method using the same according to the present invention can greatly improve the polycrystalline silicon production capacity by operating the fluidized bed reactor at high pressure.

1 and 2 show a cross-sectional view of a fluidized bed reactor for producing particulate polysilicon according to an embodiment of the present invention.
Figure 3 shows a perspective view of a heating apparatus according to an embodiment of the present invention.

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. First of all, it should be noted that in the drawings, the same components or parts denote the same reference numerals as much as possible. In describing the present invention, detailed descriptions of related well-known functions or configurations are omitted in order not to obscure the subject matter of the present invention.

As used herein, the terms "about", "substantially", and the like, are used at, or in close proximity to, numerical values as are indicative of preparation and material tolerances inherent in the meanings mentioned, and are intended to be accurate or to facilitate understanding of the invention. Absolute figures are used to prevent unfair use by unscrupulous infringers.

The flow gas used in the present invention refers to a gas supplied so that a fluidized bed constituting a bed of silicon particles is formed at the top of the chamber.

The reaction gas used in the present invention refers to a gas containing a silicon component as a raw material gas used for producing polycrystalline silicon particles.

The process of producing polycrystalline silicon using the fluidized bed reactor according to the present invention, the closed chamber to block the space from the outside; A tubular heating device located inside the chamber; A flow gas first supply pipe formed under the chamber to supply the flow gas into the heating device; And a venturi to increase the flow gas velocity inside the heater. In the fluidized bed reactor consisting of a cone for guiding silicon formed of particles, the lower part of the chamber injects a fluid gas and a reaction gas separately to form a fluidized bed in the upper part of the heating device, which is the chamber, to react. When the silicon precipitated by the reaction reaches a certain size, the weight of the silicon increases, and the silicon is lowered to the lower part of the chamber by gravity. The lowered silicon is collected through the cone, and particles of a certain size are collected under the first supply pipe, and the remainder is passed through the venturi to the fluidized bed again.

Alternatively, the chamber may be formed in a cone shape without separately configuring the cone.

EMBODIMENT OF THE INVENTION Hereinafter, this invention is demonstrated in detail with reference to drawings.

1 and 2 show a cross-sectional view of a fluidized bed reactor for producing particulate polysilicon according to an embodiment of the present invention.

Fluidized bed reactor according to an embodiment of the present invention is composed of a chamber 110, heating device 120, Venturi 150, cone 160, the first supply pipe 130, the second supply pipe 180, the third supply pipe 140, the reaction gas supply pipe 170, the discharge means 190. .

The chamber 110 is closed to block the space from the outside, and as shown in FIGS. 1 and 2, the chamber 110 upper space preferably has a larger space than the lower space to facilitate the formation of the reaction fluidized bed 10. Non-limiting examples of the material of the chamber 110 may be a metal that can be used for water-cooling (water-cooling), alloys, ceramics, and the like, more specifically, stainless-steel , Quartz and carbon steel can be used. In addition, the chamber inner wall is a surface that can be exposed to silicon seed particles and the like, the coating or lining selected from the group consisting of silicon itself, silicon carbide (SiC), silicon nitride (Si 3 N 4 ), Si 3 O 4, etc. Can be.

Figure 3 shows a perspective view of a heating apparatus according to an embodiment of the present invention.

The heating device 120 has a hollow tube shape and is installed vertically in the chamber 110. The heating device 120 includes a heating part 121, a reflecting surface 122, and an insulator 123. The heating unit 121 of the heating device 120 is preferably a halogen lamp or a graphite resistive heater. The reflective surface 122 serves to reflect the heat generated from the heater to the inside of the tube shape.

In addition, the insulator 123 surrounds the heater 121 from the outside to prevent the heat of the heater 121 from dissipating toward the chamber 110 and to transmit heat only to the inside of the heater 120. In addition, the heating unit 121 of the heating apparatus 120 may be connected to an AC or DC power supply to supply power. It is preferable that the material of the insulator 123 is not easily deformed at a high temperature. Non-limiting examples of the material of the insulator 123 include ceramics, fabrics made of silica fibers, silicon carbide (SiC), and silicon nitride (Si 3 N 4). ) Can be made. Refrasil may be used as a specific example of the fabric made of silica fibers.

In the heating apparatus, it should be noted that a predetermined space is formed between the cone 160 (the lower chamber of the chamber when no cone is formed (see FIG. 2)) and the heating apparatus 120, so that the silicon particles precipitated between the spaces are formed in the first supply pipe 130. To move to.

The cone 160 is formed to be inclined to descend to the first supply pipe 130 when the silicon particles precipitated through the fluidized bed reaction are lowered to the lower portion of the chamber 110 through the outside of the heating apparatus 120 under heavy load. The inclination of the cone 160 is not particularly limited, and it is preferable to incline 30 to 60 degrees from the horizontal plane.

The first supply pipe 130 supplies a flow gas to move the heat inside the heating apparatus 120 to the fluidized bed 10 above the chamber 110, and at the same time, when the precipitated silicon particles descending through the cone 160 are light in weight, they move back to the fluidized bed 10. Play a role. That is, when the precipitated silicon particles reach the first supply pipe 130, they are affected by the flow gas supplied from the first supply pipe 130, and when the precipitated silicon particles have a predetermined size or more, they are collected through the first supply pipe 130. It serves as a passage for selecting and collecting the silicon particles so that it can be.

As the flow gas, it is preferable to use one or more selected from hydrogen, argon and helium.

When the size of the precipitated silicon particles that are dropped through the cone 160 is small, the liquid may be accumulated in the heating unit 121 while being heated by the heating unit 121 of the heating apparatus 120 while moving back to the fluidized bed 10 by the flow gas supplied from the first supply pipe 130. However, the supply rate of the fluidized bed and the silicon particles precipitated by the Venturi 150 move rapidly in the heating apparatus 120, so there is very little concern about accumulation in the heating unit 121.

In addition, the flow gas can also be supplied through the second supply pipe 180, the flow gas supplied through the second supply pipe 180 maintains the fluidized bed 10 so that the reaction in the fluidized bed 10 is sufficiently made, precipitated to a certain size due to the reaction Among the silicon particles, the small particles are prevented from descending the chamber 110 in the fluidized bed 10.

Therefore, the fluidized bed reactor according to the present invention has the advantage of controlling the particle size of the desired polycrystalline silicon by controlling the speed of the flow gas supplied from the first supply pipe 130 and the second supply pipe 180.

In addition, the second supply pipe 180 may be formed in the lower portion of the chamber 110 outside the heating device 120 to supply the flow gas to the upper portion of the chamber 110. The flow gas supplied through the second supply pipe 180 allows the fluidized bed 10 to be formed in the upper portion of the chamber 110 and prevents the precipitated silicon of a predetermined size or less from falling down and exists in the fluidized bed 10.

The second supply pipe 180 may be provided with one or several second supply pipe 180 in the lower portion of the chamber 110 outside the heating device 120 to supply the flow gas.

In addition, the third supply pipe 140 is located above the first supply pipe 130 and the inlet venturi 150 may further supply the flow gas. As the flow gas is further supplied by using the third supply pipe 140, the moving speed increases in the heating apparatus 120, so that the movement of the particles in the fluidized bed 10 is a fraction of the spout in the direction of the arrow shown in FIGS. 1 and 2. Will move. Therefore, most of the silicon particles precipitated in the fluidized bed 10 are lowered into the space between the heater 120 and the chamber 110 outer surface rather than descending through the tube inside the heater 120 when lowered.

In addition, the venturi 150 is present inside the heating apparatus 120, and the moving speed of the flow gas supplied from the first supply pipe and the third supply pipe 140 by the venturi 150 may be further increased. When the silicon particles lowered into the chamber 110 are smaller than the desired size, the venturi 150 may effectively raise the silicon particles when the silicon particles are not lowered to the first supply pipe 130 and are raised again by the supplied flow gas.

The Venturi 150 has a horizontal cut surface that is circular, and the diameter of the circular shape decreases toward the middle portion. That is, the diameter of the middle part is smaller than the diameter of the inlet of the Venturi 150. When the flow gas flows, the pressure of the middle part is lower than the inlet pressure of the Venturi 150 so that the silicon particles at the inlet side are effectively sucked into the middle part of the Venturi 150 and the chamber 110 Move to the top of the

On the other hand, the reaction gas supply pipe 170 is located at a position higher than the heating device 120 may supply a reaction gas containing a silicon component to the upper chamber 110. The reaction gas may be used only as a silicon component, or may be used by adding one or more gas components among hydrogen, argon and helium. In addition, the reaction gas may not only provide the silicon precipitation raw material, but also contribute to the flow of the silicon particles together with the flowing gas. The proportion of the silicon component in the reaction gas is preferably 5 to 100 mol%. In the present invention, the silicon component used as the reaction gas may be selected from one or more of monosilane (SiH 4 ), dichlorosilane (SiH 2 Cl 2 ), trichlorosilane (SiHCl 3 ), tetrachloride (SiCl 4 ), and the like.

Supply of the reaction gas may be supplied in the form of spraying through a nozzle (nozzle), etc., it is preferable to spray in the direction of the fluidized bed from the top of the chamber to maintain the fluidized bed 10 well. The reaction gas may be supplied toward the fluidized bed at the top of the chamber and below the fluidized bed, or may be supplied downward toward the fluidized bed at the upper part of the chamber above the fluidized bed. The reaction gas supply pipe 170 may supply one or several reaction gas supply pipes 170 at a position higher than the heating device 120 to supply the reaction gas.

On the other hand, the flowing gas and the unreacted gas passing through the fluidized bed 10 above the chamber 110 may be discharged through the discharge means 190 as waste gas, and the discharge means 190 constantly discharges the flow gas and the reaction gas to the chamber 110. It regulates the air pressure and allows the gas to be supplied continuously. The unreacted silicon seed particles which may be discharged together with the unreacted silicon seed particles from the gas discharged through the discharge means 190 may be re-introduced through another passage of the discharge means 190 as shown in FIGS. 1 and 2. . The gaseous materials used in the flow gas and the reaction gas may be supplied again after purification. In addition, the unreacted silicon seed particles may be prevented from passing through the discharge means 190 to be treated.

Meanwhile, in order to supply seed to the fluidized bed, silicon seed particles may be supplied from the upper portion of the chamber toward the fluidized bed (not shown). The size of the seed particles is preferably 0.1 ~ 2.0mm, more preferably 0.3 ~ 1.2mm.

The silicon seed particles may be supplied to the fluidized bed by forming a separate supply means at the top of the chamber, or may be supplied to another passage that is re-introduced into the discharge means 190. In the case of forming and supplying a separate supply means, the silicon seed particles may be supplied toward the fluidized bed at the top of the chamber and below the fluidized bed, or may be supplied downward from the upper part of the chamber above the fluidized bed to the fluidized bed.

In addition, since the chamber 110 is heated while the fluidized bed reactor is operating, the outer surface of the chamber 110 uses cooling materials such as water, oil, gas, air, etc. for the purpose of protecting the reactor apparatus and workers, preventing thermal expansion, and other accidents. It is preferable to maintain the temperature below a certain temperature range. For this purpose, it is preferable to design and manufacture the circulation of the cooling fluid on the outer wall of the chamber 110. In addition, instead of the cooling, it is also possible to further install a heat insulating material on the outer surface of the chamber 110 to protect the worker and to prevent excessive heat loss.

In addition, an observation unit (not shown) may be included in the upper part of the chamber 110 to observe the reaction progress while the fluidized bed reactor is in operation, and may include a thermocouple such as a thermo-couple or pyrometer to measure temperature. can do.

In addition, the fluidized bed reactor according to the present invention does not limit the pressure in the chamber 110, so the pressure in the chamber 110 can be adjusted according to the intention of the operator, and the silicon precipitation reaction is possible at a high pressure, thereby greatly improving the production capacity. . The preferred pressure in the chamber 110 is preferably 1 to 20 bar, more preferably 3 to 6 bar, but is not limited thereto. Pressure relief valves can also be installed for emergencies.

It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the spirit or scope of the inventions. It will be clear to those who have knowledge of.

Claims (38)

In the fluidized bed reactor for producing particulate polysilicon in which a flow gas is injected from the lower part of the chamber and a reaction gas is injected into the upper part of the chamber, whereby a reaction occurs in the upper part of the chamber.
Hermetic chamber;
A tubular heating device located inside the chamber;
A flow gas first supply pipe formed under the chamber to supply the flow gas into the heating device; And
Fluidized bed reactor for producing a particulate polysilicon, characterized in that it comprises a venturi to increase the flow gas velocity inside the heater. The method of claim 1,
The fluidized bed reactor for producing particulate polysilicon, characterized in that it further comprises a cone leading the silicon formed of particles in the chamber to the first supply pipe. The method of claim 1,
The lower portion of the chamber is a fluidized bed reactor for producing a particulate polysilicon, characterized in that formed in a cone shape to guide the silicon formed of particles to the first supply pipe. 4. The method according to any one of claims 1 to 3,
A fluidized bed reactor for producing particulate polysilicon, characterized in that it comprises a reaction gas supply pipe for supplying a reaction gas containing a silicon component to the upper portion of the chamber at a position higher than the heating device. 4. The method according to any one of claims 1 to 3,
A fluidized bed reactor for producing particulate polysilicon, characterized in that to form a second supply pipe in the lower portion of the chamber outside the heating device to supply the flow gas to the upper chamber. 4. The method according to any one of claims 1 to 3,
Fluidized bed reactor for producing particulate polysilicon, characterized in that it further comprises a third supply pipe for supplying a flow gas to increase the speed of the material flowing through the venturi. 4. The method according to any one of claims 1 to 3,
Silicon seed particles are supplied through a supply means, wherein the silicon seed particles are supplied toward the fluidized bed from the bottom of the fluidized bed or from the top of the fluidized bed. 4. The method according to any one of claims 1 to 3,
The reaction gas is a fluidized bed reactor for producing a particulate polycrystalline silicon, characterized in that the silicon component or at least one of hydrogen, argon and helium in the silicon component. The method of claim 8,
The silicon component is a fluidized bed reactor for producing particulate polycrystalline silicon, characterized in that at least one selected from monosilane (SiH 4 ), silane dichloride (SiH 2 Cl 2 ), trichlorosilane (SiHCl 3 ) and tetrachloride (SiCl 4 ). The method of claim 6,
The flow gas is a fluidized bed reactor for producing particulate polysilicon, characterized in that at least one selected from hydrogen, argon and helium. 4. The method according to any one of claims 1 to 3,
The material of the chamber is a fluidized bed reactor for producing particulate polycrystalline silicon, characterized in that any one of stainless steel, quartz and carbon steel. 4. The method according to any one of claims 1 to 3,
The inner wall of the chamber is a fluidized bed reactor for producing particulate polysilicon, characterized in that coated or lined with any one of silicon, silicon carbide (SiC), silicon nitride (Si 3 N 4 ), Si 3 O 4 . 4. The method according to any one of claims 1 to 3,
The heating device is installed vertically in the lower portion of the chamber, the fluidized bed reactor for producing a particulate polysilicon, characterized in that the lower space there is a space for the silicon particles and gas to pass through. 4. The method according to any one of claims 1 to 3,
The heating device comprises a heating part, a reflecting surface and an insulator, wherein the heating part is located inside the tubular shape so that heat can be transferred to the upper part of the chamber through the inside of the heating device. . The method of claim 14,
The insulator is formed outside the tubular shape, and the material of the insulator is any one of ceramic, fabric made of silica fibers, silicon carbide (SiC) and silicon nitride (Si 3 N 4 ). Fluidized bed reactor for producing polycrystalline silicon. 4. The method according to any one of claims 1 to 3,
Fluidized bed reactor for producing particulate polysilicon, characterized in that the flowing gas and the reaction gas introduced into the chamber is discharged through the discharge means. The method of claim 16,
The silicon seed particles discharged through the discharge means are selected in size and re-introduced into the chamber, the fluidized bed reactor for producing particulate polysilicon. The method of claim 16,
The discharge means is a fluidized bed reactor for producing particulate polysilicon, characterized in that located above the chamber. 4. The method according to any one of claims 1 to 3,
Fluidized bed reactor for producing particulate polysilicon, characterized in that the pressure in the chamber is 1 to 20bar. Hermetic chamber; A tubular heating device located inside the chamber; A flow gas first supply pipe formed under the chamber to supply the flow gas into the heating device; And in the fluidized bed reactor comprising a venturi to increase the flow gas velocity inside the heater,
Particle polycrystalline silicon, characterized in that the reaction gas and the flow gas is injected separately and the silicon grown by precipitation after the fluidized layer is formed in the upper portion of the heating device, the chamber is lowered to the lower portion of the chamber to be sorted / discharged through the first supply pipe. Manufacturing method. The method of claim 20,
And a cone for guiding silicon formed of particles in the chamber to the first supply pipe. The method of claim 20,
And the chamber lower portion is formed in a cone shape to guide silicon formed of particles to the first supply pipe. The method according to any one of claims 20 to 22,
Particle polysilicon manufacturing method comprising a reaction gas supply pipe for supplying a reaction gas containing a silicon component to the upper portion of the chamber at a position higher than the heating device. The method according to any one of claims 20 to 22,
Particle polysilicon manufacturing method, characterized in that for supplying the flow gas to the upper chamber by forming a second supply pipe in the lower chamber outside the heating device. The method according to any one of claims 20 to 22,
Particle polysilicon manufacturing method further comprises a third supply pipe for supplying a flow gas to increase the speed of the material flowing through the venturi. The method according to any one of claims 20 to 22,
Particle polycrystalline silicon production method characterized in that the silicon seed particles are injected into the fluidized bed of the upper chamber. The method according to any one of claims 20 to 22,
The reaction gas is a silicon component or a method for producing particulate polycrystalline silicon, characterized in that at least one of hydrogen, argon and helium contained in the silicon component. The method of claim 27,
The silicon component is a method for producing particulate polysilicon, characterized in that at least one selected from monosilane (SiH 4 ), disilane (SiH 2 Cl 2 ), trichlorosilane (SiHCl 3 ) and tetrachloride (SiCl 4 ). The method according to any one of claims 20 to 22,
The flow gas is particulate polysilicon manufacturing method characterized in that at least one selected from hydrogen, argon and helium. The method according to any one of claims 20 to 22,
The material of the chamber is stainless-steel (stainless-steel), particulate polysilicon manufacturing method, characterized in that any one of quartz and carbon steel. The method according to any one of claims 20 to 22,
The inner wall of the chamber is a granular polysilicon manufacturing method, characterized in that the coating or lining with any one of silicon, silicon carbide (SiC), silicon nitride (Si 3 N 4 ) and Si 3 O 4 . The method according to any one of claims 20 to 22,
The heating device is installed vertically to the lower portion of the chamber, the particulate polysilicon manufacturing method, characterized in that there is a space through which the silicon particles and gas can pass. The method according to any one of claims 20 to 22,
The heating device comprises a heating unit, a reflecting surface and an insulator, wherein the heating unit is located inside the tubular shape is formed so that heat can be transferred to the upper chamber through the inside of the heating apparatus. The method of claim 33, wherein
The insulator is formed outside the tubular shape, and the material of the insulator is any one of ceramic, fabric made of silica fibers, silicon carbide (SiC) and silicon nitride (Si 3 N 4 ). Polysilicon production method. The method according to any one of claims 20 to 22,
The flow gas and the reaction gas introduced into the chamber is a particulate polysilicon manufacturing method characterized in that the discharge through the discharge means. 36. The method of claim 35,
The silicon seed particles discharged through the discharge means are selected in size and re-introduced into the chamber. 36. The method of claim 35,
The discharge means is a particulate polysilicon manufacturing method, characterized in that located above the chamber. The method according to any one of claims 20 to 22,
The pressure in the chamber is a granular polysilicon manufacturing method, characterized in that 1 to 20bar.
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KR101615307B1 (en) * 2013-07-16 2016-04-25 웅진에너지 주식회사 Polysilicon production apparatus
KR20170070005A (en) * 2014-08-15 2017-06-21 알이씨 실리콘 인코포레이티드 Segmented silicon carbide liner
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