KR102012898B1 - Apparatus and Method for producing polycrystalline silicon using multi-way feeding - Google Patents

Apparatus and Method for producing polycrystalline silicon using multi-way feeding Download PDF

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KR102012898B1
KR102012898B1 KR1020150088841A KR20150088841A KR102012898B1 KR 102012898 B1 KR102012898 B1 KR 102012898B1 KR 1020150088841 A KR1020150088841 A KR 1020150088841A KR 20150088841 A KR20150088841 A KR 20150088841A KR 102012898 B1 KR102012898 B1 KR 102012898B1
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South Korea
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gas
reaction tube
center
reaction
flow path
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KR1020150088841A
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Korean (ko)
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KR20170000097A (en
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장은수
김유석
김정규
유진형
이정우
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주식회사 엘지화학
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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
    • B01J12/00—Chemical processes in general for reacting gaseous media with gaseous media; Apparatus specially adapted therefor
    • B01J12/005—Chemical processes in general for reacting gaseous media with gaseous media; Apparatus specially adapted therefor carried out at high temperatures, e.g. by pyrolysis
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/02—Silicon
    • C01B33/021—Preparation
    • C01B33/027—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
    • C01B33/029—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition of monosilane
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/02—Silicon
    • C01B33/021—Preparation
    • C01B33/027—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
    • C01B33/03—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition of silicon halides or halosilanes or reduction thereof with hydrogen as the only reducing agent

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

Abstract

According to the present invention, a reaction tube having a reaction space therein; A center supply nozzle disposed at an upper center of the reaction tube to supply the first gas inclined toward the inner surface of the reaction tube; At least one peripheral supply nozzle disposed along the inner periphery of the reaction tube at the top of the reaction tube and capable of supplying a second gas onto the inner surface of the reaction tube; And a heating unit disposed outside the reaction tube to heat the reaction tube.

Description

Reaction apparatus for polysilicon production using multi-directional feeding and polysilicon production method thereby {Apparatus and Method for producing polycrystalline silicon using multi-way feeding}

The present invention relates to a reaction apparatus for producing silicon and a method for producing silicon thereby.

Conventionally, apparatuses and methods for producing polysilicon used as raw materials for semiconductor or photovoltaic cells are known. For example, polysilicon may be manufactured using the Siemens method, but the Siemens method uses a bell jar type reactor. In the Siemens method, the silane-based gas as the raw material gas and the hydrogen gas as the reducing gas are added together to the vertical reactor, and the heat of the silicon rod installed in the vertical reactor is heated to transfer the heat above the precipitation temperature of silicon to the reaction gas and the reducing gas. Polysilicon precipitates by reaction.

On the other hand, in the case of using a vertical reduction reactor, the source gas and the reducing gas are injected into the reaction tube and then transferred to the reaction surface to reach the target temperature on the reaction surface. In this process, if the high temperature region is included in the space that must pass before reaching the reaction surface, the reaction between the gases can occur. The main reactions and side reactions generated at this time generate silicon and by-products. The silicon is not adsorbed on the inner surface of the reaction tube and is suspended in the space inside the reaction tube by the flow of gas and is exhausted. This not only reduces the silicon conversion efficiency, but also causes damage to the exhaust line. The by-products also reduce the silicon conversion efficiency.

1 shows an apparatus for producing high purity polycrystalline silicon disclosed in Patent No. 10-1345641.

Referring to the drawings, the reactor 1 of the silicon manufacturing apparatus includes a silicon chloride gas supply nozzle 2, a reducing agent gas supply nozzle 3, and an exhaust gas leak pipe installed under the reactor 1. The reactor 1 is heated to a high temperature, and silicon is formed by reacting the silicon chloride gas and the reducing agent gas supplied through the respective supply nozzles 2 and 3 in the reactor 1.

As disclosed in the above patent document, silicon is produced by agglomerating tubularly at the tip of the chloride gas supply nozzle 2. That is, tubular aggregated polycrystalline silicon is grown downward at the nozzle tip. This method has a problem that since the growth of silicon is made only at the tip of the chloride gas supply nozzle 2, the yield efficiency of silicon cannot be increased.

It is an object of the present invention to provide an improved reaction apparatus for producing silicon and a method for manufacturing the same, which can solve the above problems of the prior art.

Another object of the present invention is to provide a reaction apparatus for producing silicon and a method for producing the same, which can improve the conversion efficiency of silicon and increase the yield.

It is another object of the present invention to provide a reaction apparatus for producing silicon and a method for producing the same, in which gas mixing and reaction can be generated at an optimal place inside the reaction tube.

In order to achieve the above object, according to the present invention,

A reaction tube having a reaction space therein;

A center supply nozzle disposed at an upper center of the reaction tube to supply the first gas inclined toward the inner surface of the reaction tube;

At least one peripheral supply nozzle disposed along the inner periphery of the reaction tube at the top of the reaction tube and capable of supplying a second gas onto the inner surface of the reaction tube; And,

There is provided a reaction apparatus for producing silicon, including a heating unit disposed outside the reaction tube to heat the reaction tube.

According to one feature of the invention, it further comprises a projection formed on the inner surface of the reaction tube, the first gas and the second gas is scattered by the projection.

According to another feature of the invention, a second gas supplied from said at least one peripheral supply nozzle is directed towards the inner surface of said reaction tube.

According to another feature of the invention, the peripheral supply nozzle may be capable of supplying a second gas in the entire inner surface in a circle along the circumference of the reaction tube.

According to another feature of the invention, the first gas is a reducing gas and the second gas is a raw material gas; The first gas is a source gas and the second gas is a reducing gas; The first gas is a reducing gas and the second gas includes a raw material gas and a reducing gas; Alternatively, the first gas includes a source gas and a reducing gas, and the second gas is a reducing gas.

According to another feature of the invention, the reducing gas is hydrogen, and the source gas is one of monosilane, dichloride, trichloride (TCS), tetrachloride.

According to another feature of the invention, the center supply nozzle is constituted by a conduit having a center conduit with a center flow path formed therein and at least one inclined flow path formed inclined with respect to the center flow path so as to be in communication with the center flow path.

According to another feature of the invention, the center supply nozzle is constituted by a central conduit with a central flow path formed therein and one or more individual conduits formed with an inclined flow path inclined with respect to the central conduit and in communication with the central flow path.

Moreover, according to this invention, the silicon manufacturing method using the reaction apparatus for silicon manufacturing is provided.

According to the reaction apparatus and manufacturing method for producing silicon using the multi-directional feed of the present invention, since the reaction of the raw material gas and the reducing gas is mainly generated on the inner surface of the reaction tube which is relatively superior to other places in the reaction tube, the conversion efficiency This can be improved and the yield of silicon can be increased. In addition, since the amount of gas that is not converted and suspended is reduced, the amount of exhaust discharged through the exhaust line is also reduced, thereby reducing side effects such as damage to the exhaust line.

1 is a schematic perspective view of an apparatus for producing silicon according to the prior art.
2 is a schematic configuration diagram of a reaction apparatus for producing silicon using a multi-directional supply according to the present invention.
3A is a detailed perspective view of the center supply nozzle shown in FIG. 2.
3B is a perspective view of another embodiment of a center supply nozzle.
4 is a schematic cross-sectional view of a reaction apparatus for producing silicon using a multidirectional feed according to the present invention.

Hereinafter, with reference to the embodiments of the present invention shown in the accompanying drawings will be described in more detail. However, this is not intended to limit the present invention to specific embodiments, it should be understood to include all modifications, equivalents, or substitutes included in the spirit and scope of the present invention.

Similar reference numerals are used for similar elements in the respective drawings.

The terms first, second, A, B, etc. may be used to describe various components, but the components are not limited by the terms, but for the purpose of distinguishing one component from another component. Only used.

The term “and / or” includes any one or a combination comprising any of the plurality of listed items.

When a component is referred to as being “connected” or “connected” to another component, it is to be understood that the other component may be directly connected or connected to or in between.

Singular expressions include plural expressions unless otherwise specified.

The terms “comprises” or “having” and the like refer to the presence of features, values, steps, operations, components, parts, or combinations thereof described in the specification and other features, values, steps, It does not exclude the possibility that an operation, component, part, or combination thereof may be present or added.

2 shows a schematic configuration diagram of a reaction apparatus for producing silicon according to the present invention.

Referring to the drawings, the reaction apparatus for producing silicon using the multi-directional supply according to the present invention is disposed in the reaction tube 21, the upper center of the reaction tube 21 is a first gas to the inner surface of the reaction tube 21 A center supply nozzle 22 capable of supplying inclined toward the inclined side and one disposed along the inner periphery of the reaction tube at the top of the reaction tube 21 to supply a second gas onto the inner surface of the reaction tube 21. The above peripheral supply nozzle 23 is provided. In addition, a heating unit 25 for heating the reaction tube 21 may be disposed around the reaction tube 21.

In the example shown in the figure, one central supply nozzle 22 is provided and four peripheral supply nozzles 23 are provided at intervals of 90 degrees along the sectional circumference of the reaction tube 21. However, in other examples not shown in the figures, more than one center feed nozzle 22 may be provided, or more than four peripheral feed nozzles or two or three peripheral feed nozzles may be provided. That is, according to one embodiment, the peripheral supply nozzle may enable the second gas supply in the entire inner surface in a circle along the circumference of the reaction tube.

In the drawing, the reaction tube 21 is shown as being open at the top for convenience of description, but in fact, the upper and lower portions of the reaction tube 21 are sealed to form a sealed reaction space therein, and the center supply nozzle 22 And one or more peripheral supply nozzles 23 are installed at the top in the internal reaction space of the reaction tube 21. In addition, although not shown in the drawing, by installing an exhaust pipe on the side or bottom of the reaction tube 21, it is possible to discharge the gas generated after the reaction in the reaction tube 21. In addition, a collection vessel for collecting the reaction product may be configured under the reaction tube 21.

Inclined to the center supply nozzle 22 so that the first gas supplied through the center supply nozzle 22 can be directed toward the inner surface of the reaction tube 21 without being fed vertically downward of the reaction tube 21. It is preferable that a flow path is formed. An exemplary configuration of the center supply nozzle 22 will be described later in more detail.

The second gas supplied through the one or more peripheral supply nozzles 23 is supplied vertically down the reaction tube 21 or toward the inner surface of the reaction tube 21. Since the peripheral supply nozzle 23 is disposed along the inner circumference adjacent to the inner surface of the reaction tube 21, the second gas flows down substantially on the inner surface of the reaction tube 21.

Accordingly, the flow of the second gas flowing downward along the inner surface of the reaction tube 21 and the flow of the first gas flowing obliquely toward the inner surface of the reaction tube 21 from the upper center of the reaction tube 21. Is encountered on the inner surface of the reaction tube 21. The reaction between the first gas and the second gas is substantially generated on the inner surface of the reaction tube 21, and the reaction at a portion other than the inner surface of the reaction tube 21 is suppressed. Since the inner surface of the reaction tube 21 is adjacent to the heating unit 25 as compared to other parts of the reaction tube 21, it can be said that the conditions for the reaction are relatively good.

In another example, the second gas supplied from the peripheral supply nozzle 23 is directed toward the inner surface at a position adjacent to the inner surface of the reaction tube 21. For example, the peripheral supply nozzle 23 is inclined at a position adjacent to the inner surface of the reaction tube 21 so that the supply direction of the second gas is at an acute angle with the vertical direction of the inner surface of the reaction tube 21. Accordingly, the second gas discharged from the peripheral supply nozzle 23 can flow down along the inner surface after being diffused while impinging on the inner surface. By adjusting the flow rate of the second gas, it is then desirable to minimize the amount of gas that is repelled after the second gas impinges on the inner surface.

The first gas that may be supplied through the central supply nozzle 22 may be a reducing gas, and the second gas that may be supplied through the peripheral supply nozzle 23 may be a source gas. The reducing gas that can be used in the production of silicon can be hydrogen. Raw material gases that can be used for the production of silicon include, for example, silane-based gases, such as monosilane, dichloride, trichloride (TCS), tetrachloride, and the like.

In another example, it is understood that the first gas that may be supplied through the central supply nozzle 22 may be a source gas, and that the second gas that may be supplied through the peripheral supply nozzle 23 may be a reducing gas. Should be. In another example, the first gas can be a reducing gas, and the second gas can include a reducing gas and a source gas together, and in another example the first gas includes a reducing gas and a source gas together and the second gas May be a reducing gas.

For example, the first gas and the second gas may be supplied at a temperature of about 100 to 200 ° C., and the temperature of the reaction tube may be heated to 1200 ° C. to 1600 ° C. or more.

FIG. 3A is a detailed perspective view of the center supply nozzle shown in FIG. 2, and FIG. 3B is a perspective view of another embodiment of the center supply nozzle.

Referring to FIG. 3A, the center supply nozzle 22 has a center conduit in which a center flow path 31 is formed and a conical portion joined to a lower portion of the center conduit, and a plurality of inclined flow paths 32 are formed in the cone. do. The inclined flow path 32 is formed to be inclined with respect to the vertical direction. Each inclined flow path 32 is connected to be in communication with the central flow path 31, the lower end of the inclined flow path 32 corresponds to the discharge port 33. The inclined flow path 32 is formed in the cone so that the center supply nozzle 22 is directed toward the inner surface of the reaction tube 21 when the center supply nozzle 22 is installed in the center at the top of the reaction tube 21. The first gas is introduced into each inclined flow path 32 through the central flow passage 31, and the first gas discharged through the respective discharge ports 33 is the reaction tube 21 as described with reference to FIG. 2. Can be directed towards the inner surface of the.

Referring to FIG. 3B, the center supply nozzle 22 ′ has a center conduit 31 ′ and one or more individual conduits 32 ′ extending while forming an obtuse angle with respect to the center conduit 31 ′. The flow path formed in the central conduit 31 'is connected with the flow path formed in the individual conduit 32'. When the center supply nozzle 22 'is installed in the center at the top of the reaction tube 21 shown in FIG. 2, the center supply nozzle (1) is directed so that the individual conduits 32' are directed toward the inner surface of the reaction tube 21. 22 ') is installed.

4 is a schematic cross-sectional view of a reaction apparatus for producing silicon according to the present invention.

Referring to the drawings, as described with reference to FIG. 2, a central supply nozzle 22 and one or more peripheral supply nozzles 23 are arranged on top of the reaction tube 21. The flow of the first gas discharged from the center supply nozzle 22 and the flow of the second gas discharged from the peripheral supply nozzle 23 are indicated by arrows, respectively. It is preferable that the protrusion 41 is formed where the flow of a 1st gas and the flow of a 2nd gas meet. The projection 41 scatters the flow of gas, whereby the mixing of the first gas and the second gas can be made smoothly, thus allowing the reaction to be made relatively active. That is, the projection 41 performs a gas mixing function. The protrusion 41 may be formed on the entire inner surface of the reaction tube 21 or may be partially formed.

Although the present invention has been described with reference to the embodiments shown in the accompanying drawings, this is merely exemplary, and it will be understood by those skilled in the art that various modifications and equivalent other embodiments are possible. There will be. Therefore, the true scope of protection of the present invention should be defined only by the appended claims.

21. Reaction tube 22. Center supply nozzle
23. Ambient supply nozzle 25. Heating section
32. Inclined flow path 22 'center supply nozzle

Claims (9)

A reaction tube having a reaction space therein;
A center supply nozzle for injecting a first gas from the upper center of the reaction tube to the surface of the inner sidewall of the reaction tube at an angle formed at an acute angle to the longitudinal direction of the reaction tube;
It is provided on the upper part of the reaction tube while injecting the second gas from the upper portion of the reaction tube in parallel with the longitudinal direction of the reaction tube so that the second gas flows along the surface of the inner side wall of the reaction tube A peripheral feed nozzle closer to the upper edge of the reaction tube than to the upper center of the reaction tube;
And a heating unit disposed outside the reaction tube to heat the reaction tube. The method of claim 1,
And a projection formed on the surface of the inner sidewall of the reaction tube, wherein the first gas and the second gas are scattered by the projections. delete The method of claim 1,
The peripheral supply nozzle is to enable a second gas supply throughout the surface of the inner side wall in a circular shape along the circumference of the reaction tube, polysilicon production reactor. The method of claim 1,
The first gas is a reducing gas and the second gas is a raw material gas;
The first gas is a source gas and the second gas is a reducing gas;
The first gas is a reducing gas and the second gas includes a raw material gas and a reducing gas; or
Reaction apparatus for producing polysilicon, wherein the first gas comprises a source gas and a reducing gas and the second gas is a reducing gas. The method of claim 5,
The reducing gas is hydrogen, and the raw material gas is monosilane, dichloride, trichloride (TCS), tetrachlorosilane is a reaction apparatus for producing polysilicon. The method of claim 1,
And the center supply nozzle is constituted by a conduit having a center conduit in which a center flow path is formed and at least one inclined flow path formed to be inclined with respect to the center flow path so as to be in communication with the center flow path. The method of claim 1,
Wherein said center supply nozzle is comprised by a central conduit with a central flow path formed therein and one or more individual conduits formed with an inclined flow path inclined relative to said central conduit and in communication with said central flow path. A method for producing polysilicon using the reaction apparatus for producing polysilicon according to any one of claims 1, 2 and 4 to 8.
KR1020150088841A 2015-06-23 2015-06-23 Apparatus and Method for producing polycrystalline silicon using multi-way feeding KR102012898B1 (en)

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EP3763673B1 (en) * 2018-04-05 2023-04-19 Tokuyama Corporation Polycrystalline silicon rod manufacturing method, and reactor
CN109592686B (en) * 2018-12-21 2019-10-25 亚洲硅业（青海）有限公司 Adjusting method for the feed pipe of reduction furnace, reduction furnace and feed pipe aperture

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KR20120086422A (en) * 2011-01-26 2012-08-03 주식회사 케이씨씨 Distribution apparatus of fluidized bed reactor producing granulated polysilicon
KR101298233B1 (en) * 2011-03-08 2013-08-22 주식회사 케이씨씨 Fluidized bed reactor for producing a granulated polysilicon
KR101626645B1 (en) * 2013-08-14 2016-06-01 주식회사 엘지화학 Apparatus for producing polysilicon and preparation of polysilicon using same

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