KR20160124519A - Horizontal Type Reactor For Producing Polycrystalline Silicon - Google Patents
Horizontal Type Reactor For Producing Polycrystalline Silicon Download PDFInfo
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- KR20160124519A KR20160124519A KR1020150055243A KR20150055243A KR20160124519A KR 20160124519 A KR20160124519 A KR 20160124519A KR 1020150055243 A KR1020150055243 A KR 1020150055243A KR 20150055243 A KR20150055243 A KR 20150055243A KR 20160124519 A KR20160124519 A KR 20160124519A
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- reaction tube
- circular plane
- reaction
- tube member
- silicon
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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
- 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
- B01J8/36—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 through which there is an essentially horizontal flow of particles
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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
- B01J8/1836—Heating and cooling the reactor
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/021—Preparation
- C01B33/027—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
- C01B33/035—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition or reduction of gaseous or vaporised silicon compounds in the presence of heated filaments of silicon, carbon or a refractory metal, e.g. tantalum or tungsten, or in the presence of heated silicon rods on which the formed silicon is deposited, a silicon rod being obtained, e.g. Siemens process
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- 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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- Combustion & Propulsion (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
Description
The present invention relates to a horizontal reaction apparatus for manufacturing polysilicon, and more particularly, to a horizontal reaction apparatus for producing silicon having a reaction tube for allowing a raw material gas and a reducing gas to flow in a horizontal direction.
Polysilicon is a raw material for semiconductor devices, solar cell devices, and the like. Conventionally, various methods for producing silicon used as a raw material for a semiconductor or a solar cell have been known, and some of them have already been carried out industrially.
Most of the currently used high purity polysilicon is produced by a chemical vapor deposition method. Can be prepared by reacting a trichlorosilane gas with a reducing gas such as hydrogen gas, specifically as shown in Reaction Scheme 1 below.
[Reaction Scheme 1]
SiHCl 3 (gas) + H 2 (gas) → Si (solid) + 3HCl (gas)
An example of a commercialized process for producing polysilicon is the Siemens method. In the Siemens method, a bell jar type reactor is used. In the Siemens method, a silane-based gas as a raw material gas and hydrogen gas as a reducing gas are introduced together into a vertical reactor, and when a heat of more than a silicon deposition temperature is transferred to the reaction gas and the reducing gas by heating the silicon rod installed in the vertical reactor, Polysilicon is precipitated by the reaction. However, the bell-shaped reactor used in the Siemens method has a problem that the energy consumption is very large and the deposition efficiency is small, and the facility investment cost is high.
Another method is the precipitation by a fluidized bed. This method is a method of continuously producing silicon grains of 1 to 2 mm by depositing silicon on fine silicon particles by supplying silane streams while supplying fine grains of about 100 microns into the precipitation nuclei by using a fluidized bed. This method has an advantage of being able to operate for a relatively long period of time. However, since monosilane having a low precipitation temperature is used as a raw material for silicon, generation of fine silicon by thermal decomposition of monosilane and precipitation of silicon into the reactor wall are likely to occur even at a relatively low temperature Periodic cleaning or replacement of the reaction vessel is necessary.
On the other hand, in the case of using the vertical reduction reactor, the raw material 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. The raw gas and the reducing gas react with the thermal energy of the reaction surface to produce a polysilicon liquid and move to the lower end of the reactor.
Figure 1 shows a schematic illustration of a reactor for making silicon according to the prior art.
Referring to FIG. 1, a
In the reactor for producing silicon shown in FIG. 1, an attempt was made to smooth the mixing of the gas or to expand the reaction area in order to increase the chance of reacting the raw gas with the reducing gas. For example, a constant flow pattern, such as a vortex, can be imparted to the flow of gas so that the feed gas and the reducing gas are mixed smoothly in the reactor. It is also possible to give the reaction surface a predetermined shape or to form an obstacle in order to expand the reaction area inside the reactor.
However, such technical attempts cause other problems. For example, in order to impart a flow pattern to the flow of the gas, the configuration and arrangement of the gas injection nozzle become complicated, thereby making the configuration of the entire reactor difficult. Also, when an obstacle is formed on the reaction surface, so-called dead volume is formed incidentally, and by-products and products are deposited on the dead volume, which is a cause of lowering the efficiency of the reaction.
On the other hand, US Patent 6,784,079 B2 discloses a method for producing silicon. The U.S. Patent describes a reactor for producing silicon, which is a vertical reactor in which the gas fed through the feed port flows from top to bottom.
SUMMARY OF THE INVENTION It is an object of the present invention to provide a horizontal reactor for improved silicon production capable of solving the problems of the prior art as described above.
Another object of the present invention is to provide a horizontal reaction device for silicon production having a horizontal reaction tube in which the efficiency of obtaining silicon can be improved by enlarging the reaction area.
Another object of the present invention is to provide a horizontal type reaction device for silicon production capable of reducing facility investment costs.
In order to achieve the above object, according to the present invention, there is provided a horizontal reaction device for silicon production, comprising a horizontal reaction tube in which one or more reaction tubes of a truncated cone shape having an inlet diameter larger than an outlet diameter are connected.
According to one aspect of the present invention, the horizontal reaction tube comprises a reaction tube member having a truncated cone shape having an outer circumferential surface extending between a first circular plane and a second circular plane having different diameters, As a result,
Wherein the central axis of each of the reaction tube members extends in a straight line and is disposed horizontally,
A flange formed at an edge of a second circular plane of one reaction tube member and a flange formed at an edge of a first circular plane of another adjacent reaction tube member are bonded to each other, And the first circular plane of the other reaction tube member have different diameters,
At least one of the plurality of reaction tube members may be formed with an opening formed by removing an outer circumferential surface.
According to another aspect of the present invention, the flange provided in the first circular plane of each of the plurality of reaction tube members is provided with at least one rod made of silicon or silicon carbide, and heat is generated by applying current to the rod.
According to another aspect of the present invention, the opening portion is formed to face downward in the vertical direction.
According to another aspect of the present invention, the first circular plane of one of the reaction tube members disposed at the outermost side of the reaction tube for producing silicon is closed, a gas inlet is formed in the closed first circular plane, The second circular plane of the other one of the reaction tube members disposed on the outermost side of the production reaction tube is closed and the gas exhaust port is formed in the second circular plane closed.
According to another aspect of the present invention, the reaction tube members can be heated by providing an electric coil on the outer peripheral surface of at least one of the reaction tube members.
According to another aspect of the present invention, one or more rods provided in a first circular plane of one reaction tube member protrude through a hole formed in a flange provided in a second circular plane of another adjacent reaction tube member.
According to another aspect of the present invention, the apparatus may further include a collecting unit disposed below the reaction tube for producing silicon and collecting the molten silicon falling through the opening.
According to the present invention, there is also provided a process for producing polysilicon using the reaction apparatus.
In the horizontal reaction apparatus for manufacturing silicon according to the present invention, the size of the reaction tube inlet can be easily controlled and the initial reaction can be smoothly induced. Also, since the raw material gas can actively contact the reaction surface and / or the rod in the horizontal reaction tube, the silicon conversion rate is increased. Also, the inner surface temperature of the reaction tube or the temperature of the rod can be appropriately controlled, so that it is easy to control the silicon conversion characteristic according to the temperature. On the other hand, since the molten silicon can be supplied to the post-process in a molten state without cooling, energy loss required for re-melting can be reduced. On the other hand, the reaction tube for silicon production according to the present invention and the horizontal type reaction apparatus for silicon production having the same have the advantage of being easy to manufacture and low in manufacturing cost.
BRIEF DESCRIPTION OF DRAWINGS FIG. 1 is a schematic view showing a schematic configuration of a reactor for producing silicon according to the prior art; FIG.
Fig. 2 is an overall configuration diagram of a horizontal reaction apparatus for producing silicon according to the present invention.
FIGS. 3 and 4 show the results of computational simulation of the reaction behavior in an ideal plug flow reactor (PFR).
FIG. 5 is a schematic exploded perspective view of a horizontal reaction tube included in the horizontal type reaction apparatus for producing silicon according to the present invention shown in FIG. 2. FIG.
FIG. 6 is a configuration diagram showing the structure of a horizontal reaction tube according to the present invention shown in FIG.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will now be described in detail with reference to the embodiments of the present invention shown in the accompanying drawings. It is to be understood, however, that the invention is not to be limited to the specific embodiments, but includes all modifications, equivalents, or alternatives falling within the spirit and scope of the present invention.
In the drawings, like reference numerals are used for similar elements.
The terms first, second, A, B, etc. may be used to describe various components, but the components are not limited by these terms, and may be used to distinguish one component from another Only.
The term " and / or " includes any one or a combination of the plurality of listed items.
It is to be understood that when an element is referred to as being "connected" or "connected" to another element, it is to be understood that other elements may be directly connected or connected, or intervening elements may be present.
The singular expressions include plural expressions unless otherwise specified.
It will be understood that the terms "comprises", "having", and the like have the same meanings as the features, numbers, steps, operations, elements, parts or combinations thereof described in the specification, Does not exclude the possibility that an operation, component, component, or combination thereof may be present or added.
Fig. 2 is an overall configuration diagram of a horizontal reaction apparatus for producing silicon according to the present invention.
Referring to the drawings, a horizontal type reaction apparatus for producing silicon according to the present invention includes a
The reaction gas which has not yet reacted in the
Assuming that the steady-state isothermal reaction (T 0 ) proceeds in an ideal flood flow reactor for the horizontal reaction tube as shown in FIG. 2, the mass balance equation for the molar flow rate can be established as follows.
V is the volume (m 3 ), F is the molar flow (mol / s)
FIGS. 3 and 4 show the results of computer simulation of the reaction in the reactor according to the above conditions, respectively.
FIG. 3 shows the case where the reaction tube volume is 5.0 x 10 -4 m 3 , the temperature is 1,703 K, trichlorosilane (TCS) is 12 g / min, and H 2 is 29 nl / min. 60 g / min of trichlorosilane (TCS), and 100 nl / min of H 2 .
The left and right graphs of FIGS. 3 and 4 are shown separately due to the molar flow scale difference. In Fig. 4, Cl2 shows a molar flow scale which is not shown in the graph and has a value of 4.5 x 10 -5 mol / s.
3 and 4, it can be seen that the amount of TCS is reduced and the amount of HCl, Cl, and SiCl is increased while entering the high-temperature region at the beginning of the reaction starting material, and TCS -> SiCl 2 -> Si It can be seen that an explosive reaction occurs in the early stage.
As a result, it can be seen that the improvement of the silicon conversion efficiency can be expected by increasing the volume of the reaction tube inlet. The inventors of the present invention have made the present invention based on this fact. That is, according to the present invention, one or more reaction tubes of a truncated cone shape having an inlet diameter larger than the outlet diameter may be connected to form a horizontal reaction tube so as to increase the space at the inlet of the reaction tube.
FIG. 5 is a schematic exploded perspective view illustrating an embodiment of a horizontal reaction tube included in the horizontal type reaction apparatus for manufacturing silicon according to the present invention shown in FIG. FIG. 6 is a configuration diagram showing the structure of a horizontal reaction tube according to the present invention shown in FIG.
Referring to the drawings, the structure of the
As is known, a 'truncated cone' is defined as a solid that excludes a three-dimensional object including a vertex from among two solid objects formed by cutting into a plane parallel to the bottom surface of the conical shape. The truncated cone thus has a first circular plane and a second circular plane with different diameters and an outer circumferential surface extending between the first plane and the second plane.
Each of the first to sixth
The first circular plane of one of the two outermost two reaction tube members and the second plane of the other reaction tube member are closed while the first circular plane and the second circular plane of the other reaction tube members are both closed Lt; / RTI > That is, the first circular plane of the first
The first
The first circular plane of the first
The second
The second
The second
The third
A
The fourth
The fifth
The sixth reaction tube member (36) is bonded to the second circular plane of the fifth reaction tube member (35) in a first circular plane. The diameter of the first circular plane of the sixth reaction tube member (36) is smaller than the diameter of the second circular plane of the fifth reaction tube member (35). The diameter of the first circular plane of the sixth reaction tube member (36) is larger than the diameter of the second circular plane of the sixth reaction tube member (36). The first circular plane of the sixth
Referring to FIG. 6, it is understood that the
When the
Although an example of a reaction tube composed of the first to sixth reaction tube members in the embodiment shown in the drawings has been described, it should be understood that this is merely exemplary. That is, a reaction tube having a different number of reaction tube members is possible, for example, a reaction tube made up of fewer than six or more than six reaction tube members can be realized. It should also be understood that a horizontal reaction tube without a rod can be realized.
While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is evident that many alternatives, modifications and variations will be apparent to those skilled in the art. There will be. Accordingly, the true scope of protection of the present invention should be determined only by the appended claims.
20.
23.
31.32.33.34.35.36. The reaction tube member
Claims (9)
1. A reaction tube for producing silicon, which is constituted by mutually joining reaction tube members in a truncated cone shape having an outer circumferential surface extending between a first circular plane and a second circular plane having different diameters,
Wherein the central axis of each of the reaction tube members extends in a straight line and is disposed horizontally,
A flange formed at an edge of a second circular plane of one reaction tube member and a flange formed at an edge of a first circular plane of another adjacent reaction tube member are bonded to each other, And the first circular plane of the other reaction tube member have different diameters,
Wherein at least one of the plurality of reaction tube members is provided with an opening formed by removing an outer circumferential surface thereof.
Characterized in that at least one rod made of silicon or silicon carbide is provided on the flange provided in the first circular plane of each of the plurality of reaction tube members and heat is generated by applying current to the rod, Reaction device.
Wherein the opening is formed so as to face downward in the vertical direction.
Wherein the first circular plane of one of the reaction tube members disposed on the outermost side of the reaction tube for producing silicon is closed and the gas inlet is formed in the closed first circular plane,
Characterized in that the second circular plane of the other one of the reaction tube members disposed at the outermost side of the reaction tube for producing silicon is closed and the gas exhaust is formed in the closed second circular plane, Device.
Wherein the reaction tube members can be heated by providing an electric coil on the outer circumferential surface of at least one of the reaction tube members.
Wherein at least one rod provided in the first circular plane of one reaction tube member protrudes through a hole formed in a flange provided in a second circular plane of the adjacent another reaction tube member.
Further comprising a collecting portion disposed below the horizontal reaction tube for collecting molten silicon falling through the opening portion.
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Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH10287413A (en) * | 1997-02-13 | 1998-10-27 | Mitsui Chem Inc | Production apparatus of polycrystal silicon |
US20030119284A1 (en) * | 2001-06-06 | 2003-06-26 | Satoru Wakamatsu | Method of manufacturing silicon |
JP2007519592A (en) * | 2003-11-21 | 2007-07-19 | スタットオイル エイエスエイ | Method |
KR20090017634A (en) * | 2006-06-02 | 2009-02-18 | 우데 인벤타-피셔 게엠바하 | End reactor |
KR20100101302A (en) * | 2009-03-09 | 2010-09-17 | (주)룩스이엔지 | Apparatus and method of manufacturing polysilicon |
JP2014088275A (en) * | 2012-10-29 | 2014-05-15 | Tokuyama Corp | Method for producing polycrystalline silicon |
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2015
- 2015-04-20 KR KR1020150055243A patent/KR101955287B1/en active IP Right Grant
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH10287413A (en) * | 1997-02-13 | 1998-10-27 | Mitsui Chem Inc | Production apparatus of polycrystal silicon |
US20030119284A1 (en) * | 2001-06-06 | 2003-06-26 | Satoru Wakamatsu | Method of manufacturing silicon |
JP2007519592A (en) * | 2003-11-21 | 2007-07-19 | スタットオイル エイエスエイ | Method |
KR20090017634A (en) * | 2006-06-02 | 2009-02-18 | 우데 인벤타-피셔 게엠바하 | End reactor |
KR20100101302A (en) * | 2009-03-09 | 2010-09-17 | (주)룩스이엔지 | Apparatus and method of manufacturing polysilicon |
JP2014088275A (en) * | 2012-10-29 | 2014-05-15 | Tokuyama Corp | Method for producing polycrystalline silicon |
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