KR20140018460A - Apparatus for producing granular polycrystalline silicon - Google Patents

Apparatus for producing granular polycrystalline silicon Download PDF

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Publication number
KR20140018460A
KR20140018460A KR1020120080276A KR20120080276A KR20140018460A KR 20140018460 A KR20140018460 A KR 20140018460A KR 1020120080276 A KR1020120080276 A KR 1020120080276A KR 20120080276 A KR20120080276 A KR 20120080276A KR 20140018460 A KR20140018460 A KR 20140018460A
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chamber
silicon
manufacturing apparatus
particle
polycrystalline silicon
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KR1020120080276A
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Korean (ko)
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임천수
박윤석
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(주)기술과가치
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    • 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
    • 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
    • C30B28/00—Production of homogeneous polycrystalline material with defined structure
    • C30B28/12—Production of homogeneous polycrystalline material with defined structure directly from the gas state
    • C30B28/14—Production of homogeneous polycrystalline material with defined structure directly from the gas state by chemical reaction of reactive gases
    • 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

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  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Combustion & Propulsion (AREA)
  • General Chemical & Material Sciences (AREA)
  • Silicon Compounds (AREA)

Abstract

The present invention relates to an apparatus for producing granular polycrystalline silicon. More specifically, the present invention relates to an apparatus for producing granular polycrystalline silicon capable of realizing a complete continuous process without generating precipitate on the inner wall of a reactor. The flow layer of seed particles is formed under high pressure. A reaction gas is supplied to precipitate metal silicon on the seed particles. A previously-selected high purity granular polycrystalline silicon with a constant size is manufactured.

Description

Apparatus for Producing Granular Polycrystalline Silicon}

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an apparatus for producing particulate polycrystalline silicon, and more particularly, in the preparation of particulate polycrystalline silicon, to effectively prevent deposition and accumulation of metal silicon in the reactor wall and heating portion, and continuously The present invention relates to a particulate polysilicon production apparatus capable of operating in a process as well as uniformly selecting particle sizes and producing high purity silicon particles.

In order to produce polycrystalline silicon, a Siemens Chemical Vapor Deposition (CVD) process is generally used in which a silicon component is deposited on a seed silicon surface by pyrolysis or hydrogen reduction of a reaction gas containing a silicon component. However, this method is low productivity as a batch process.

In addition, the vertical reactor used in the Siemens process is an electric resistance heating method, which limits the diameter of the rod that increases due to the precipitation of silicon. Consumption has a very big disadvantage.

Therefore, in order to solve this disadvantage, recently, a silicon deposition process using a fluidized bed reaction that enables continuous production of particulate polycrystalline silicon has been developed. According to this method, the silicon particles in the fluidized bed (fluidized bed) by the flow gas in the reactor, the silicon component in the reaction gas precipitates on the surface of these silicon particles heated to a high temperature to grow the particles to produce a polycrystalline silicon product do. At this time, the small size silicon seed particles (種 粒子, seed crystal, 0.5 ~ 4.0mm diameter) is lost due to gravity due to the continuous precipitation of the silicon component to sink to the bottom of the fluidized bed. The product particles thus grown are discharged to the product collection container, and the particles which do not grow to a certain size are continuously introduced into the fluidized bed and continue to precipitate / grow. At the same time, silicon seed particles are continuously introduced 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 the advantage that the surface area of the silicon particles that can be precipitated is large, the reaction yield is high under the same reaction conditions, the power consumption is greatly reduced and the reaction can be maintained continuously.

However, silicon-containing gases such as silane (SiH 4 ) , silane dichloride (SiH 2 Cl 2 ) , trichlorosilane (SiHCl 3 ) and tetrachloride silane (SiCl 4 ) decompose themselves above about 300 ° C. (initial decomposition temperature) to form homogeneous particles. It is easy to cause not only homogeneous nucleation but also agglomeration precipitation, and metallic silicon (different from “organic silicon”) is deposited on the surface of the inner wall of the fluidized bed reactor where the reaction temperature is higher than the initial decomposition temperature regardless of the material type of the surface. do. Accordingly, not only silicon precipitation occurs on the surface of the flowing silicon particles, but also metal silicon precipitates accumulate in the reactor inner wall.

Accumulation of the inner wall of the reactor of such silicon precipitates not only lowers the yield of the product, but also prevents continuous operation of the fluidized bed reactor due to generation of particles or chunks out of specification. In addition, the accumulation of silicon precipitates inside the reactor may not only cause breakage or degradation of the reactor and safety problems, but also may cause physical or thermal deformation of the precipitate layer or mass, which may cause cracking or breakage in the reactor. The risk of accidents is very high.

In Korean Patent No. 10-0411180, "Method and Apparatus for Manufacturing Polycrystalline Silicon", a large-scale production of particulate polycrystalline silicon using a fluidized bed reactor is provided by using a nozzle for supplying an etching gas containing hydrogen chloride. Although a method and apparatus for producing polycrystalline silicon are disclosed to efficiently prevent the deposition and accumulation of silicon on the surface of a reaction gas supply means and to operate the reactor continuously, the process of etching with hydrogen chloride Corrosion of the product polycrystalline silicon to reduce the yield and there is a disadvantage that additional process is required additionally.

In addition, US Pat. No. 7029632 discloses that a heating unit is disposed outside the reaction tube and at the same time is disposed in the vicinity of the heating zone without directly contacting the reaction tube to heat the silicon particles above the reaction temperature by radiant heat in the heating zone. It is characterized by. However, the patent causes a problem that the silicon accumulates in the inner reaction tube in contact with the heating portion.

When the metal silicon accumulates as described above, it is necessary to stop the continuous process and remove the metal silicon accumulated on the inner wall, thereby causing a decrease in productivity. 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, there has been a need for the development of a technology that enables continuous operation by minimizing the accumulation of silicon on the reactor wall during the production of polycrystalline silicon particles.

In addition, since the particle size of the product discharged from the fluidized bed is not fractionated, it is difficult to select the particles to be recovered and used as seed particles, and it is troublesome to produce a product having a constant particle distribution through a separate process. At the same time, when silane is used as a reaction gas, there is a problem in that the yield is lowered due to homogeneous nucleation or agglomeration of particles.

In addition, there is a disadvantage in that the particle distribution of the product is widened because there is no size sorting device of the falling particles grown by the precipitation reaction, and in order to solve this problem, a separate seed particle selection and product collection process is required to reduce the productivity. There is a problem.

An object of the present invention to solve the above problems is to provide a continuous fluidized bed reactor for producing particulate polysilicon that can prevent metal silicon from accumulating on the inner wall of the reaction zone of the heating zone and the reaction zone.

Another object of the present invention is to provide a production apparatus for producing high purity polycrystalline silicon particles.

Another object of the present invention to provide a polysilicon production apparatus that can be carried out in a completely continuous process in the production of polycrystalline silicon particles.

Still another object of the present invention is to provide a manufacturing apparatus capable of producing polysilicon particles having a narrow particle size distribution.

In order to achieve the above object, the present invention provides a fluidized bed reactor for producing particulate polysilicon, in which a flow gas and a reaction gas are injected and a reaction occurs at the top, the chamber comprising: a closed chamber; A reaction zone located above the chamber a heating zone located below the chamber; A cone collecting particulate polycrystalline silicon under the heating zone of the chamber; A particle sorting tube connected to the chamber for supplying a particle size sorting gas to the chamber to sort the size of the polycrystalline silicon; And a collecting part connected to the chamber, wherein the inside of the chamber and the collecting part operate under the same pressure to provide a granular polycrystalline silicon manufacturing apparatus in which a product is collected at the same time as silicon production.

In another aspect, the present invention provides a heating device is formed in the heating zone, the heating unit is provided in close contact with the lower inner wall of the chamber to provide a particulate polysilicon manufacturing apparatus.

The present invention also provides an apparatus for producing particulate polysilicon having a reaction zone cross-sectional area equal to or less than 15% of the heating zone cross-sectional area.

In another aspect, the present invention provides a particulate polysilicon manufacturing apparatus, characterized in that the heating unit is made of a heater, a reflecting surface and an insulator, the heat generated in the heating unit is transferred to the reaction zone of the upper chamber through the flow gas.

In addition, the present invention is the heating portion is in close contact with the chamber and cooled with argon.

In another aspect, the present invention provides an apparatus for producing particulate polycrystalline silicon, characterized in that the material of the insulator is any one of a ceramic, a fabric made of silica fibers and silicon carbide (SiC).

In another aspect, the present invention provides a particulate polycrystalline silicon production apparatus, characterized in that the cross-sectional area is gradually smaller from the top to the bottom, the top cross-sectional area of the particle sorting tube is 1 to 10% larger than the bottom cross-sectional area.

In another aspect, the present invention is characterized in that the first valve is formed between the particle separator and the collecting unit, the first valve is opened during the production of the granular polycrystalline silicon, and is closed when the particulate polycrystalline silicon is discharged from the collecting unit. Provided is a particulate polycrystalline silicon manufacturing apparatus.

In addition, the present invention is that the hopper connected to the second valve is formed in the lower portion of the collector, the second valve is opened after the first valve is closed to move the polycrystalline silicon of the collector and at the same time the reaction is performed in a continuous process in the chamber An apparatus for producing a particulate polycrystalline silicon is provided.

In another aspect, the present invention provides a granular polysilicon production apparatus characterized in that the locking dock is formed that the collector and the hopper can lower the product in a sealed connection.

In another aspect, the present invention provides a device for producing particulate polysilicon, characterized in that the pressure of the hopper is equal to or lower than the reaction pressure in the chamber, the pressure of the hopper is 1 to 10% lower than the pressure in the chamber.

In another aspect, the present invention provides an apparatus for producing particulate polysilicon having a side surface of the collector portion and a cone shape at the bottom thereof.

In another aspect, the present invention provides a particulate polysilicon manufacturing apparatus, characterized in that the pressure in the chamber is precipitated by 1 ~ 20bar.

In another aspect, the present invention can supply a flow gas in the vicinity of the cone shape, the flow gas provides a particulate polysilicon manufacturing apparatus, characterized in that at least one selected from hydrogen, argon and helium.

In another aspect, the present invention provides a particulate polysilicon manufacturing apparatus comprising a reaction gas supply pipe for supplying a reaction gas containing a silicon component toward the reaction zone at a position higher than the heating zone.

The present invention also provides an apparatus for producing particulate polysilicon, wherein the reaction gas is contained in at least one of hydrogen, argon and helium in the silicon component or the silicon component.

In another aspect, the present invention is the production of particulate polycrystalline silicon, characterized in that at least one selected from silane (SiH 4 ), silane dichloride (SiH 2 Cl 2 ), trichloride (SiHCl 3 ) and tetrachloride (SiCl 4 ). Provide a device.

In another aspect, the present invention provides a particulate polysilicon manufacturing apparatus characterized in that the flow gas supply pipe is formed in the vicinity of the cone shape of the lower chamber to supply the flowing gas to the upper chamber.

In another aspect, the present invention provides a particulate polysilicon production apparatus, characterized in that the silicon seed particles are introduced from the bottom to the reaction zone.

In another aspect, the present invention provides a particulate polysilicon production apparatus, characterized in that the silicon seed particles are screened by a cyclone separator is introduced from the top.

In another aspect, the present invention provides a granular polysilicon production apparatus made of a stainless steel (steel).

In another aspect, the present invention provides an apparatus for producing particulate polysilicon, wherein the chamber is formed in duplicate to maintain the temperature of the inner wall of the cooling water at a temperature at which the reactants containing the silicon component do not vaporize or precipitate.

In another aspect, the present invention provides an apparatus for producing particulate polysilicon, characterized in that the inner wall of the chamber using high-purity metal silicon itself, or coated or lined with silicon carbide (SiC).

In another aspect, the present invention provides an apparatus for producing particulate polysilicon, characterized in that the particle size sorting gas, the flowing gas and the reaction gas introduced into the chamber is discharged through a cyclone separator.

In another aspect, the present invention provides an apparatus for producing particulate polysilicon, characterized in that the outside of the chamber is packaged with an insulator.

The particulate polysilicon manufacturing apparatus according to the present invention does not occur in the accumulation of metal silicon on the inner wall increases the yield and at the same time enable a continuous reaction to increase the yield.

In addition, the granular polysilicon production apparatus according to the present invention has a further effect that productivity is improved because it does not need to interrupt the process because it enables the continuous supply of seed particles.

In addition, the granular polysilicon production apparatus according to the present invention can operate the reactor even at high pressure, thereby greatly improving productivity.

In addition, the apparatus for producing particulate polycrystalline silicon according to the present invention enables the production of particulate polycrystalline silicon having a desired particle distribution by controlling the speed of the particle size sorting gas supplied to the collecting port and designing the particle sorting tube.

Figure 1 shows a cross-sectional view of the particulate polysilicon manufacturing 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, it should be noted that the same constituent elements or parts in the drawings denote the same reference numerals as much as possible. In the following description of the present invention, a detailed description of known functions and configurations incorporated herein will be omitted so as to avoid obscuring the subject matter of the present invention.

As used herein, the terms "substantially", "substantially", and the like are used herein to refer to a value in or near the numerical value when presenting manufacturing and material tolerances inherent in the meanings mentioned, Absolute numbers are used to prevent unauthorized exploitation by unauthorized intruders of the mentioned disclosure.

The flow gas used in the present invention refers to a gas supplied to form a reaction zone for allowing silicon particles to grow through the reaction to form polycrystalline silicon.

Reaction gas used in the present invention is a raw material gas used in the production of polycrystalline silicon particles containing a silicon component (silane (SiH 4 ), dichlorosilane (SiH 2 Cl 2 ), trichlorosilane (SiHCl 3 ) and Silane tetrachloride (SiCl 4 )).

Figure 1 shows a cross-sectional view of the particulate polysilicon manufacturing apparatus according to an embodiment of the present invention.

The chamber is closed to block the space from the outside, and as shown in FIG. 1, the chamber upper space has a smaller space than the lower heating zone to facilitate the formation of the reaction zone 10.

The present invention relates to an apparatus for producing particulate polycrystalline silicon, comprising: an enclosed chamber; A reaction zone located above the chamber; A heating zone located below the chamber; A cone collecting particulate polycrystalline silicon under the heating part of the chamber; A particle sorting tube connected to the chamber for supplying a particle size sorting gas to the chamber to sort the size of the polycrystalline silicon; And a collecting part connected to the chamber, wherein the inside of the chamber and the collecting part are operated under the same pressure, so that the product is collected at the same time as the manufacture of silicon and the continuous process is possible.

Referring to FIG. 1, the apparatus for manufacturing polycrystalline silicon according to an exemplary embodiment of the present invention may include a chamber 110, a reaction zone 10, a heating zone 20, and a particle sorting tube 140.

In addition, a first valve 150 may be formed between the particle sorting tube 140 and the collecting unit 160.

The chamber is closed to block the space from the outside, and as shown in FIG. 1, the chamber upper space preferably has a larger space than the lower space in order to facilitate the formation of the reaction zone 10. In addition, the horizontal cross section of the chamber is preferably circular.

In the polycrystalline silicon manufacturing apparatus according to the present invention, a process of continuously manufacturing polycrystalline silicon is as follows.

Depending on the operation, the silicon seed particles of similar size may be provided from near the shape of the cone 130 under the heating zone 20, or the silicon seed particles included in the exhaust gas may be selected and re-introduced into an appropriate size with a cyclone separator.

The seed particles used in the present invention are seed particles selected by a cyclone separator or seed particles introduced near the bottom cone shape.

When the silicon seed particles float into the reaction zone 10 through the heating zone 20 in the form of a fluidized bed, they meet with the reaction gas containing silicon and precipitate on the surface of the seed particles. It descends to (130) direction.

The final product classified in the particle sorting tube 140 is collected by the collecting unit due to gravity, but the particles smaller than the standard is floated back into the reaction zone 10 through the heating zone 20 again by the particle size sorting gas. The floating small particles stay in the reaction zone until they reach a suitable size through the precipitation reaction. In addition, the particle sorting tube 140 is connected to the collecting unit 160 through the first valve so that the polycrystalline silicon particles are collected into the collecting unit by gravity. Therefore, the pressure in the chamber and the pressure in the collecting part can continuously proceed at the same pressure.

In addition, the polycrystalline silicon manufacturing apparatus of the present invention has an advantage in that even if the polycrystalline silicon is almost filled in the collecting unit 160, the polycrystalline silicon can be continuously manufactured without stopping the process. That is, when the polycrystalline silicon is collected in the collecting unit 160 and there is no space, when the first valley unit 140 is closed and the second valve 170 is opened, the completed polycrystalline silicon moves to the hopper 180. Therefore, according to the present invention, it is possible to maintain the hermeticity with the external atmosphere while continuing the work.

The collecting unit 160 has a side surface of a cylindrical shape and a bottom of a cone shape.

In addition, the hopper 180 connected to the collecting unit 160 may be formed as a closed locking dock 181. Since the locking dock is formed, the collector 160 and the hopper 180 may be lowered in a sealed state. The moving operation from the collecting unit 160 to the hopper 180 is easily started by opening the second valve 170 under a somewhat low pressure of the product hopper 180. More specifically, the pressure of the hopper 180 preferably forms a pressure equal to or slightly lower than the reaction pressure in the chamber to start product movement.

The pressure of the hopper is preferably about 1 to 10% lower than the pressure in the chamber.

Since the polycrystalline silicon manufacturing apparatus according to the present invention is not limited to the pressure in the chamber, the pressure in the chamber can be adjusted according to the intention of the operator, and the metal silicon precipitation rate can be improved at high pressure. More preferably, the pressure in the chamber is 20 bar or 5-6 bar at normal pressure. Pressure relief valves can also be installed for emergencies.

In the chamber, a reaction zone and a heating zone may be formed.

In addition, the flow gas supply pipe 40 is formed in the vicinity of the cone shape of the lower chamber can be supplied with the flow gas, the flow gas supplied through the flow gas supply pipe 40 is sufficiently reacted in the reaction zone (10) The reaction zone 10 is maintained so that the small sized particles of the metal silicon particles precipitated to a certain size due to the reaction do not fall to the lower part of the chamber in the reaction zone 10 and remain in the reaction zone 10. do. The flow gas supply pipe 40 may be provided at one or several flow gas supply pipes 40 in the vicinity of the cone shape to supply the flow gas.

The reactor maintains the reactor inner wall temperature at 35 ~ 300 ℃ using an external insulator.

As a non-limiting example of the material of the chamber 110 may be used as a material that can be cooled (water-cooled) using a cooling fluid such as water, but may be metal, alloy, ceramics, etc., stainless-steel ), Carbon steel and the like are preferable. All internal surfaces are preferably maintained at about 35-300 ° C. at a temperature at which the reactants do not vaporize or precipitate with cooling water.

In addition, the inner wall of the chamber may be exposed to silicon seed particles or product particles, so that the metal silicon may be precipitated. Therefore, the chamber inner wall may be coated with or coated with silicon carbide (SiC) to prevent this. Can be.

In addition, a heating part is formed in the heating zone, and the heating part may be formed in close contact with the lower inner wall of the chamber.

Preferably, the reaction zone horizontal cross-sectional area is 5 to 15% smaller than the heating zone horizontal cross-sectional area. This is because when the flow gas passes through the heating zone 20 and is transferred to the reaction zone having a small cross sectional area, as the cross sectional area becomes smaller, the velocity of the same amount of the flow gas (including the particle size sorting gas) is increased to facilitate the formation of the fluidized bed. In addition, the heating time is relatively long in the heating zone where the flow gas (including the particle size sorting gas) is slow, so that heating is effective.

The heating unit includes a heater 111, a reflective surface 122, and an insulator 123. The heater 111 of the heating unit is preferably a halogen lamp or a graphite resistance heater. The reflective surface and the reflective surface 122 allows the heat generated from the heater 111 to reflect only inside the chamber. The reflective surface may be made of silver coating.

In addition, the heating unit may be sealed with quartz or continuously cooled with argon gas.

In addition, the insulator 123 surrounds the heater 111 at an outer portion, and prevents heat of the heater 111 from being transferred to the chamber wall and allows heat to be transferred only into the chamber.

In addition, the heater of the heating unit 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 deformed at a high temperature. Non-limiting examples of the material of the insulator 123 may be made of ceramic, a fabric made of silica fibers, silicon carbide (SiC), or the like. have. Specific examples of the fabric made of silica fibers may use Refrasil or AEROGEL.

Cone 130 may be formed in the lower portion of the heating zone in the lower chamber. When large metal silicon particles formed by precipitation in the reaction zone 10 in the upper portion of the chamber descend out of the fluidized bed, the particle sorting tube 140 may be formed. It is formed to be inclined to collect. The inclination of the cone 130 is not particularly limited and is preferably inclined at 5 degrees or more from the horizontal plane. When the size of the precipitated silicon particles having passed through the shape of the cone 130 below the chamber is smaller than a predetermined size, the heating zone 20 is again opened by the particle size sorting gas 30 supplied to the particle sorting tube 140. It moves to the reaction zone 10 through.

In addition, the particle sorting tube 140 supplies a particle size sorting gas 30 to assist in moving the heat inside the heating unit 120 to the heating zone 20 of the upper chamber. However, when the precipitated silicon particles reach the particle separation pipe 140, the particle size selection gas 30 supplied from the particle separation pipe 140 is affected, and when the precipitated silicon particles become more than a predetermined size. Pass through the particle sorting tube 140 to be collected in the collecting unit 160.

The particle sorting pipe may have a cross-sectional area that gradually increases from the bottom to the top, and the top cross-sectional area of the particle sorting pipe is 1 to 10% larger than the bottom cross-sectional area.

The particle sorting tube may collect particles having a desired size as the cross-sectional area gradually increases from the bottom to the top. The shape of the particle sorting tube is a device for more precisely distinguishing small particles that have not been sorted at the top. This determines the particle size distribution depending on the content (rate) of the particle size screening gas and the design of the particle size screen.

In addition, the collecting unit 160 serves to collect polycrystalline silicon particles. A first valve is formed between the collecting unit 160 and the particle sorting tube 140 to produce the first polycrystalline silicon. A valve is opened and the first valve is closed when the particulate polycrystalline silicon is discharged from the collecting part to the product hopper. When the polycrystalline silicon is manufactured, the chamber and the collecting unit 160 are maintained at the same pressure, and when the polycrystalline silicon is manufactured, the first valve is opened to allow the process to continue in the chamber.

In addition, the hopper 180 is connected to the lower portion of the collecting unit 160, so that the polycrystalline silicon filled in the collecting unit 160 can be discharged, the connected portion of the collecting unit 160 and the hopper 180 The second valve 170 may be formed.

The first valve 150 and the second valve 170 may be operated in opposite directions to enable a continuous process. That is, when the first valve 150 is opened, the second valve 170 is closed so that the chamber and the collecting unit 160 are sealed to the outside, so that polycrystalline silicon can be continuously manufactured, and the collecting unit 160 is polycrystalline. When filled with silicon, the second valve 170 may be opened after the first valve 150 is closed to transfer the polycrystalline silicon to the hopper 180 without changing the reaction pressure of the entire chamber.

The particle size sorting gas 30 is preferably selected from one or more of hydrogen, argon and helium.

The flow gas may be the same as the particle size sorting gas, it is preferable to use at least one selected from hydrogen, argon and helium.

On the other hand, the reaction gas supply pipe (50, 51) is located at a position higher than the heating unit 120 can supply a reaction gas containing a silicon component, the reaction gas is lowered toward the reaction zone 10 in the upper chamber It may be supplied to 50, or may be supplied to the upper portion 51 toward the reaction zone 10 from the upper portion of the heating portion. The reaction gas supply pipe may use one or a plurality of supply pipes.

The reaction gas may be used only as a silicon component, or may be used by mixing 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%. The silicon component used as the reaction gas in the present invention may be used by mixing one or more of silane (SiH 4 ), dichlorosilane (SiH 2 Cl 2 ), trichlorosilane (SiHCl 3 ), tetrachloride (SiCl 4 ), and the like.

The supply of the reaction gas may be supplied in the form of spraying through the reaction gas supply pipe (50, 51) of the nozzle (nozzle) form, sprayed in the direction of the reaction zone 10 to maintain the reaction zone 10 It is desirable to be able to.

The nozzles of the reaction gas supply pipes 50 and 51 may supply argon gas to prevent silicon from depositing inside the nozzle, but may also supply a mixture of some hydrogen chloride.

In addition, the silicon seed particles may be supplied toward the reaction zone 10 at the top of the chamber or at the bottom of the heating zone to supply the silicon seed particles to the reaction zone 10.

That is, the silicon seed particles may be supplied through the seed particle supply pipe 60 near the cone 130 shape under the heating zone, and a separate supply means (not shown) is formed at the upper portion of the reaction zone 10. It can also be supplied to

The size of the silicon seed particles is typically 0.1 to 2.0 mm, but more preferably the size of the silicon seed particles is 0.3 to 1.2 mm.

Meanwhile, the flow gas, the particle size sorting gas, and the unreacted gas passing through the reaction zone 10 in the upper portion of the chamber are discharged through the cyclone separator 190 as waste gas, and the cyclone separator may be connected to the upper portion of the chamber.

In addition, unreacted silicon seed particles are screened and re-injected into a cyclone separator.

In addition, the chamber is changed to a high temperature during operation of the polycrystalline silicon manufacturing apparatus according to the present invention, the outer surface of the chamber for the purpose of preventing or protecting the device and workers, thermal expansion, and other accidents, such as water, oil, gas It is preferable to maintain the temperature below a predetermined temperature range using a cooling material such as air or the like.

To this end, it is preferable to design and manufacture the circulation of the cooling fluid to the chamber outer wall.

In addition, the outside of the chamber is preferably packaged with an insulator.

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 (25)

In the apparatus for producing a particulate polycrystalline silicon injecting a flow gas and a reaction gas, the reaction occurs at the top,
Hermetic chamber;
A reaction zone located above the chamber;
A heating zone located below the chamber;
A cone collecting particulate polycrystalline silicon under the heating zone of the chamber;
A particle sorting tube connected to the chamber for supplying a particle size sorting gas to the chamber to sort the size of the polycrystalline silicon; And
Consists of a collector connected to the chamber,
Particle polycrystalline silicon manufacturing apparatus that the product is collected at the same time as the inside of the chamber and the collecting unit under the same pressure to manufacture the silicon. The method of claim 1,
Heating unit is formed in the heating zone, the heating unit is a particulate polysilicon manufacturing apparatus, characterized in that formed in close contact with the lower inner wall of the chamber. The method of claim 1,
Particle polysilicon manufacturing apparatus, characterized in that the reaction zone cross-sectional area is 1-15% smaller than the heating zone cross-sectional area. The method of claim 1,
The heating unit comprises a heater, a reflecting surface and an insulator, wherein the heat generated from the heating unit is a particulate polysilicon manufacturing apparatus, characterized in that the transfer to the reaction zone of the upper chamber through the flow gas. 5. The method of claim 4,
The heating unit is in close contact with the chamber, the particulate polysilicon manufacturing apparatus, characterized in that for cooling with argon gas. 5. The method of claim 4,
The material of the insulator is a particulate polysilicon manufacturing apparatus, characterized in that any one of a ceramic, a fabric made of silica fibers, and silicon carbide (SiC). The method of claim 1,
The particle sorting tube has a smaller cross-sectional area from the top to the bottom, and the topmost cross-sectional area of the particle sorting tube is 1 to 10% larger than the lowest cross-sectional area of the particulate polycrystalline silicon manufacturing apparatus. The method of claim 1,
A first valve is formed between the particle sorting tube and the collecting part so that the first valve is opened when the particulate polycrystalline silicon is manufactured, and is closed when the particulate polycrystalline silicon is discharged from the collecting part. Silicon manufacturing equipment. 9. The method of claim 8,
A hopper connected to the second valve is formed below the collection part,
And a second valve is opened after the first valve is closed to move the polycrystalline silicon of the collecting part, and the reaction is performed in a continuous process in the chamber. The method of claim 1,
Particle polysilicon manufacturing apparatus, characterized in that the locking dock is formed that the collector and the hopper can lower the product by a sealed connection. 11. The method of claim 10,
The pressure of the hopper is equal to or lower than the reaction pressure in the chamber, the particulate polysilicon manufacturing apparatus, characterized in that the pressure of the hopper is 1 to 10% lower than the pressure in the chamber. The method of claim 1,
The collector is a side (cylinder) of the side (cylinder) shape, the bottom of the cone (corn) shape (particle) polysilicon manufacturing apparatus. The method of claim 1,
Particle polycrystalline silicon production apparatus, characterized in that the pressure in the chamber is precipitated by 1 ~ 20bar. The method of claim 1,
A flow gas can be supplied near the cone shape, wherein the flow gas is at least one selected from hydrogen, argon, and helium. The method of claim 1,
Particle polysilicon manufacturing apparatus characterized in that it comprises a reaction gas supply pipe for supplying a reaction gas containing a silicon component toward the reaction zone at a position higher than the heating zone. 16. The method of claim 15,
The reaction gas is a silicon component or particulate polysilicon manufacturing apparatus, characterized in that at least one of hydrogen, argon and helium contained in the silicon component. 17. The method of claim 16,
Particle polysilicon manufacturing apparatus, characterized in that at least one selected from the silane (SiH 4 ), silane dichloride (SiH 2 Cl 2 ), trichlorosilane (SiHCl 3 ) and tetrachloride (SiCl 4 ). The method of claim 1,
Particle polysilicon manufacturing apparatus, characterized in that the flow gas supply pipe is formed in the vicinity of the cone shape of the lower chamber to supply the flowing gas to the upper chamber. The method of claim 1,
Particle polysilicon manufacturing apparatus, characterized in that the silicon seed particles are introduced from the bottom to the reaction zone. The method of claim 1,
Particle polycrystalline silicon production apparatus, characterized in that the silicon seed particles in the reaction zone is screened by a cyclone separator is introduced from the top. The method of claim 1,
Particle polycrystalline silicon manufacturing apparatus of which the material of the chamber is made of stainless steel (stainless-steel). The method of claim 1,
The chamber is formed in a double, the polycrystalline silicon production apparatus for maintaining the temperature of the inner wall with the cooling water at a temperature at which the reactants containing the silicon component is not gasified or precipitated. The method of claim 1,
The inner wall of the chamber is a high-purity metal silicon itself, or granular polysilicon manufacturing apparatus, characterized in that the coating or lining with silicon carbide (SiC). The method of claim 1,
Particle size sorting gas, flow gas and reaction gas introduced into the chamber is a particulate polysilicon manufacturing apparatus, characterized in that discharged through the cyclone separator. The method of claim 1,
Particle polysilicon manufacturing apparatus, characterized in that the outside of the chamber is packaged with an insulator.
KR1020120080276A 2012-07-23 2012-07-23 Apparatus for producing granular polycrystalline silicon KR20140018460A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20170108881A (en) * 2016-03-18 2017-09-27 주식회사 엘지화학 Ultra-high temperature precipitation process for preparing polycrystalline silicon
CN109319784A (en) * 2018-11-09 2019-02-12 西安交通大学 Melt calcium carbide once cooling granulation formation system and exhaust heat recovering method
CN110172299A (en) * 2019-03-19 2019-08-27 漳州盈顺公路工程有限公司 A kind of reflective exterior coating of aqueous porcelainization and its preparation method and application
CN113897682A (en) * 2021-10-29 2022-01-07 大连弘源矿业有限公司 Polycrystalline silicon washing and selecting processing equipment

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20170108881A (en) * 2016-03-18 2017-09-27 주식회사 엘지화학 Ultra-high temperature precipitation process for preparing polycrystalline silicon
CN109319784A (en) * 2018-11-09 2019-02-12 西安交通大学 Melt calcium carbide once cooling granulation formation system and exhaust heat recovering method
CN110172299A (en) * 2019-03-19 2019-08-27 漳州盈顺公路工程有限公司 A kind of reflective exterior coating of aqueous porcelainization and its preparation method and application
CN113897682A (en) * 2021-10-29 2022-01-07 大连弘源矿业有限公司 Polycrystalline silicon washing and selecting processing equipment
CN113897682B (en) * 2021-10-29 2024-02-20 大连弘源矿业有限公司 Polysilicon washing and selecting processing equipment

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