KR101329029B1 - Fluidized bed reactor including reaction gas supplying nozzle - Google Patents

Abstract

In the fluidized bed reactor of the present invention, the reaction tube in which the precipitation of silicon occurs, the reaction gas supply nozzle for supplying the reaction gas capable of causing precipitation of the silicon to the inner space of the reaction tube, and the inert gas inactive with the silicon A fluidized bed reactor may be provided that includes one or more inert gas supply nozzles for cooling some or all of the reaction gas supply nozzles located in the interior space.

Description

FLUIDIZED BED REACTOR INCLUDING REACTION GAS SUPPLYING NOZZLE}

The present invention relates to a fluidized bed reactor, and more particularly, to a fluidized bed reactor including a reaction gas supply nozzle.

High purity polycrystalline silicon is used as a raw material for silicon single crystals for semiconductor wafers and silicon thin film materials for solar cells.

In order to manufacture polycrystalline silicon, a chemical vapor deposition (CVD) method is used in which a silicon element is continuously deposited on a silicon surface by pyrolysis or hydrogen reduction of a reaction gas containing a silicon element.

As such, for the commercial mass production of polysilicon used for semiconductor applications, bell-jar type reactors have been mainly used until now, and the diameter of polycrystalline silicon products manufactured using the reactor is about 50. It has a rod shape of ˜300 mm.

The vertical reactor, in which electric resistance heating is the core, has a limit on the diameter of the rod that increases due to the precipitation of silicon, which makes it impossible to continuously produce the product, and requires a preheating process to improve the electrical conductivity of the silicon rod at room temperature. The power consumption for maintaining the above reaction temperature on the silicon rod surface has a very big disadvantage.

In order to solve the shortcomings of the vertical reactor, a silicon precipitation process using a fluidized bed reactor capable of producing polysilicon in the form of particles has recently been developed. According to this method, a fluidized bed through which the silicon particles flow is formed by the reaction gas supplied into the reactor.

As silicon elements in the reaction gas continue to precipitate on the surface of these silicon particles heated to a high temperature, the particles become larger and larger, thereby producing a polysilicon product. At this time, as the size of the silicon seed particles (種 粒 子, seed crystal) is increased by the continuous precipitation of silicon elements, the fluidity of the silicon particles decreases and gradually sinks to the lower portion of the fluidized bed. The silicon seed particles can be continuously or periodically fed into the fluidized bed, and the silicon particles, i.e., polysilicon products, increased in size by the precipitation reaction can be withdrawn continuously or periodically from the bottom of the reactor.

The mass production of polycrystalline silicon through fluidized bed reactors has attracted much attention as the task of replacing fossil fuels causing solar pollution with solar cells has emerged.

Accordingly, fluidized bed reactor manufacturers are conducting various research activities to increase the efficiency of silicon deposition and mass production of polycrystalline silicon using a fluidized bed reactor.

At this time, since the silicon silicon precipitated in the reaction gas supply nozzle acts as a factor to inhibit the silicon deposition efficiency, there is an increasing demand for a technology for removing or reducing the silicon deposited in the reaction gas supply nozzle. In addition, in order to mass-produce polycrystalline silicon, the size of a fluidized bed reactor needs to be increased. As the size of the fluidized bed reactor increases, the demand for a technique for evenly dispersing the reaction gas in the fluidized bed reactor is increasing.

Embodiment of the present invention is to provide a fluidized bed reactor that can reduce the silicon precipitated in the reaction gas supply nozzle and provide an even distribution of the reaction gas as the size of the fluidized bed reactor increases.

According to one aspect of the invention, the reaction tube supplying the reaction of the silicon precipitation occurs, the reaction gas supply nozzle for supplying the reaction gas that can cause the precipitation of the silicon and the inert gas inert to the silicon Thus, a fluidized bed reactor including one or more inert gas supply nozzles for cooling some or all of the reaction gas supply nozzles located in the internal space may be provided.

The inert gas supply nozzle may contact part or all of an outer surface of the reaction gas supply nozzle to surround a part or all of the outer surface of the reaction gas supply nozzle.

The height of the inert gas supply nozzle may be equal to or greater than the height of the reaction gas supply nozzle.

The central axis of the inert gas supply nozzle at the end of the inert gas supply nozzle may not be parallel to the central axis of the reaction gas supply nozzle.

The inert gas supply nozzle may be spaced apart from the reaction gas supply nozzle by a predetermined distance to inject the inert gas toward the reaction gas supply nozzle.

The reaction gas supply nozzle may supply an etching gas that reacts with the silicon to remove the silicon together with the reaction gas.

The reaction gas supply nozzle may supply the reaction gas and the etching gas at the same time or at different time points.

The inert gas supply nozzle may supply an etching gas that reacts with the silicon to remove the silicon together with the inert gas.

The inert gas supply nozzle may supply the inert gas and the etching gas at the same time or at different time points.

Some of the plurality of inert gas supply nozzles supply the inert gas, and the rest may supply an etching gas that reacts with the silicon to remove the silicon along with the inert gas.

The reaction gas supply nozzle and the inert gas supply nozzle may be coaxial, and the reaction gas supply nozzle may be located inside the inert gas supply nozzle.

The reaction gas supply nozzle may have an injection unit inclined at a predetermined angle from a central axis of the reaction gas supply nozzle.

The reaction gas supply nozzle may have a single injection unit for supplying the reaction gas toward a circumference of a virtual circle perpendicular to the central axis and having a center point on the central axis.

A spiral induction line may be formed on the surface of the injection unit of the reaction gas supply nozzle to induce an outflow direction of the reaction gas.

The reaction gas may be directed in an outflow direction along the spiral induction line and discharged in a vortex form.

The reaction gas supply nozzle may have a plurality of injection parts for supplying the reaction gas in different directions.

The plurality of injection units may penetrate the inert gas supply nozzle.

The reaction gas supply nozzle may further have an injection unit for supplying the reaction gas along the central axis of the reaction gas supply nozzle.

The inert gas may include hydrogen, an inert gas, or a mixed gas of the hydrogen and the inert gas.

The temperature of the inert gas may be 600 ° C. or less.

The fluidized bed reactor further includes a body in which the reaction tube is installed therein, the body includes a first body part, a second body part and a bottom part, and the second body part is located below the first body part. It may be connected to the first body portion, the bottom portion is located below the second body portion and connected to the second body portion, the reaction gas supply nozzle and the inert gas supply nozzle may be installed.

The fluidized bed reactor further includes a body in which the reaction tube is installed therein, the body includes a first body part, a second body part and a bottom part, and the bottom part is connected to the second body part and the reaction gas A base plate on which a supply nozzle and the inert gas supply nozzle are installed, a first plate disposed on the base plate to insulate the base plate, a heater located on the first plate, and supplying heat to the internal space; And a second plate for contacting and supplying electricity to the heater, and a third plate having an insulating function to prevent contamination of the polycrystalline silicon deposited on the second plate by the second plate. have.

The fluidized bed reactor according to the embodiment of the present invention may include a reactive gas supply nozzle including an inert gas supply nozzle and inclined at a central axis to reduce silicon precipitated in the reactive gas supply nozzle, and react the reaction gas into a reaction tube. Evenly distributed in the inner space of the.

1 shows a fluidized bed reactor according to an embodiment of the present invention.
2 shows silicon precipitated in the flowing gas supply nozzle.
3 and 4 show examples of a reaction gas supply nozzle and an inert gas supply nozzle of a fluidized bed reactor according to an embodiment of the present invention.
5 shows a case where the inert gas supply nozzle does not surround the reaction gas supply nozzle.
6 shows the case where the height of the inert gas supply nozzle is smaller than the height of the reaction gas supply nozzle.
7 to 9 show other examples of the reaction gas supply nozzle and the inert gas supply nozzle of the fluidized bed reactor according to the embodiment of the present invention.
10 is a plan view of a reaction gas supply nozzle and an inert gas supply nozzle shown in FIGS. 1, 3, 4, and 7.
FIG. 11 is another plan view of the reaction gas supply nozzle and the inert gas supply nozzle shown in FIGS. 1, 3, 4, and 7.
12 shows the case where the inert gas supply nozzle is inside the reaction gas supply nozzle.
13 to 17 show other examples of the reaction gas supply nozzles shown in FIGS. 1, 3, 4, 7, 7, and 11.
18 shows a fluidized bed reactor according to another embodiment of the present invention.
19A and 19B illustrate a connection structure between a first partial reaction tube and a second partial reaction tube of the fluidized bed reactor of FIGS. 1 and 18.
FIG. 20 illustrates an assembly structure of plates and a heater of the fluidized bed reactor of FIGS. 1 and 19.

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, preferred embodiments of the present invention will be described with reference to the accompanying drawings. In describing the present embodiment, the same designations and the same reference numerals are used for the same components, and further description thereof will be omitted.

1 shows a fluidized bed reactor in an embodiment of the invention. As shown in FIG. 1, the fluidized bed reactor according to the embodiment of the present invention includes a reaction tube 110, a reaction gas supply nozzle 120, and an inert gas supply nozzle 130.

The reaction tube 110 provides an internal space 111 in which precipitation of silicon occurs. The reaction tube 110 may be in the form of a tube or may include a tube, cone and elliptical portions. The reaction tube 110 may be made of an inorganic material that is not easily deformed at a high temperature, and may include quartz, silica, silicon nitride, boron nitride, zirconia, yttria, silicon carbide, graphite, silicon, glassy carbon, or a composite thereof. It may be made of the same inorganic material. When the reaction tube 110 is made of a carbon-containing material such as silicon carbide, graphite, glassy carbon, the carbon-containing material may contaminate the polycrystalline silicon, so the inner wall surface of the reaction tube 110 may contact the polycrystalline silicon. It may be coated or lined with silicon, silica, quartz, silicon nitride and the like. At this time, the reaction tube 110 is installed inside the body 140, the body 140 protects the reaction tube 110. The body 140 may be made of a metal material having excellent mechanical strength and easy processing, such as carbon steel, stainless steel, or other alloy steel.

The reaction gas supply nozzle 120 supplies a reaction gas, which may cause precipitation of silicon, to the internal space. The reaction gas contains a silicon element component as a raw material gas used for precipitation of polycrystalline silicon. The reaction gas is monosilane (SiH ₄ ), disilane (disilane: Si ₂ H ₆ ), higher silane (Si _n H _{2n +2} , n is a natural number of 3 or more), dichlorosilane (DCS: SiH ₂ Cl ₂ ), trichloride Silane (TCS: SiHCl ₃ ), Silane tetrachloride (STC: SiCl ₄ ), Dibromosilane (SiH ₂ Br ₂ ), Tribromosilane (SiHBr ₃ ), Silicontetrabromide (SiBr ₄ ), Diiodosilane (SiH ₂ I ₂ ), triiodosilane (SiHI ₃ ) and silicontetraiodide (SiI ₄ ). At this time, the reaction gas may further include at least one of hydrogen, nitrogen, argon, helium, or hydrogen chloride.

At this time, the flow gas supply nozzle 150 supplies the flow gas to the internal space to flow the silicon seed particles. The flowing gas may include at least one of hydrogen, nitrogen, argon, helium, hydrogen chloride (HCl), and silane tetrachloride (SiCl ₄ ). Flow gas supply nozzle 150 may be a tube, a liner or a molded article made of an inorganic material, but is not limited thereto.

When the reaction gas is supplied to the silicon seed particles flowing with the supply of the flowing gas, polycrystalline silicon is deposited on the surface of the polycrystalline silicon seed particles having a size of about 0.5 to 3 mm, thereby increasing the size of the polycrystalline silicon seed particles. If the size of the polycrystalline silicon seed particles is increased to some extent, it is discharged out of the fluidized bed reactor through the polycrystalline silicon outlet (not shown).

The heater 160 supplies heat to the internal space. The heater 160 supplies heat to the inside of the reaction tube 110 for causing the silicon precipitation reaction on the surface of the polycrystalline silicon particles. The heater 160 may include at least one of graphite, ceramics such as silicon carbide, or metal materials.

One or more inert gas supply nozzles 130 supply silicon and an inert inert gas to cool some or all of the reaction gas supply nozzles 120.

Since the silicon precipitation reaction is an endothermic reaction, the heater supplies heat to the reaction tube 110. Accordingly, when the temperature of the internal space of the reaction tube 110 increases, the temperature of the reaction gas supply nozzle 120 exposed to the internal space also increases. When the reaction gas supply nozzle 120 at a high temperature supplies the reaction gas, as shown in FIG. 2, the silicon component of the reaction gas may be precipitated on the inner wall or the end of the reaction gas supply nozzle 120. Can be. Silicon formed on the inner wall or the end of the reaction gas supply nozzle 120 prevents the reaction gas from flowing out of the reaction gas supply nozzles. Accordingly, the amount of the reaction gas supplied to the internal space of the reaction tube 110 may be reduced or the reaction gas may not be constantly supplied to the internal space, thereby reducing the silicon deposition efficiency.

In an embodiment of the present invention, the one or more inert gas supply nozzles 130 supply silicon and an inert gas which is inert to cool some or all of the reaction gas supply nozzles 120. That is, the inert gas supply nozzle 130 may cool the reaction gas supply nozzle 120 by supplying an inert gas lower than the temperature of the reaction gas supply nozzle 120.

Accordingly, since the temperature of the reaction gas supply nozzle 120 is lowered, the amount of silicon deposited on the reaction gas supply nozzle 120 may be reduced or silicon may not be deposited. Etching gas (etching gas) will be described later than the inert gas to remove the silicon precipitated in the reaction gas supply nozzle 120 by reacting with the silicon.

Since the inert gas does not react with the silicon or the degree of reaction is weak, the inert gas may prevent the silicon seed particles or the polycrystalline silicon product from being contaminated by the inert gas 110. In an embodiment of the present invention, the inert gas may include hydrogen, an inert gas, or a mixed gas of hydrogen and an inert gas.

On the other hand, in order for the silicon precipitation reaction to occur, the temperature of the internal space must be 600 ° C or higher. Accordingly, when the temperature of the inert gas is 600 ° C. or less, since the temperature of the reaction gas supply nozzle 120 may not be 600 ° C. or lower or higher than 600 ° C., silicon precipitation may occur less in the reaction gas supply nozzle 120.

In the embodiment of the present invention, the inert gas supply nozzle 130 ejects the cooling gas into the inner space of the reaction tube 110, instead of circulating the cooling gas or the cooling liquid.

In order to circulate the cooling gas or the cooling liquid, the structure of the fluidized bed reactor may be very complicated. That is, in order for the cooling gas to be circulated, not only an inflow channel of the cooling gas but also a recovery channel of the cooling gas must be formed in the fluidized bed reactor. In addition, since the cooling gas takes heat from the internal space of the reaction tube 110, a high temperature cooling gas recovery apparatus may be required when recovering the cooling gas.

On the other hand, in the embodiment of the present invention, since the inert gas supply nozzle 130 ejects the cooling gas into the inner space of the reaction tube 110, the structure of the fluidized bed reactor can be prevented from becoming complicated.

Next, various examples of the reaction gas supply nozzle 120 and the inert gas supply nozzle 130 of the fluidized bed reactor according to the embodiment of the present invention will be described with reference to the drawings.

3 and 4 show examples of a reaction gas supply nozzle and an inert gas supply nozzle of a fluidized bed reactor according to an embodiment of the present invention.

As shown in FIG. 3, the inert gas supply nozzle 130 may contact all of the outer surface of the reaction gas supply nozzle 120 to surround the entire outer surface of the reaction gas supply nozzle 120. In addition, as shown in FIG. 4, the inert gas supply nozzle 130 may contact a portion of the outer surface of the reaction gas supply nozzle 120 to surround a portion of the outer surface of the reaction gas supply nozzle 120.

As shown in FIG. 5, unlike the embodiment of the present invention, unless the inert gas supply nozzle 130 ′ does not surround the reaction gas supply nozzle, the reaction gas supply nozzle region (not in contact with the inert gas supply nozzle 130 ′) Since the 510 is not cooled, the silicon 200 may be deposited in the reaction gas supply nozzle region 510. Accordingly, the reaction gas is not supplied smoothly, the silicon deposition efficiency may be reduced.

Since the inert gas supply nozzle 130 of FIGS. 3 and 4 surrounds part or all of the outer surface of the reaction gas supply nozzle 120, the area where the reaction gas supply nozzle 120 contacts the inert gas supply nozzle 130 has a large area. Can increase. Accordingly, the silicon that may be deposited on the inner surface or the end of the reaction gas supply nozzle 120 may be reduced or the silicon may not be deposited. That is, the entire or part of the reaction gas supply nozzle 120 located in the inner space of the reaction tube 110 according to the inert gas supply nozzle 130 is cooled to reduce the silicon precipitated in the reaction gas supply nozzle 120 or silicon This may not precipitate.

Meanwhile, as illustrated in FIGS. 3 and 4, the height h2 of the inert gas supply nozzle 130 may be equal to or greater than the height h1 of the reaction gas supply nozzle 120. As shown in FIG. 6, when the height h2 of the inert gas supply nozzle is smaller than the height h1 of the reaction gas supply nozzle, unlike the embodiment of the present invention, the inert gas reaches the end region of the reaction gas supply nozzle. It may be difficult to do so, and thus silicon 200 may be deposited at the end region of the reaction gas supply nozzle.

As illustrated in FIGS. 7 and 8, the height h2 of the inert gas supply nozzle 120 may be greater than the height h1 of the reaction gas supply nozzle. At this time, as shown in Figure 7, the end of the inert gas supply nozzle 130 is bent toward the central axis of the reaction gas supply nozzle 120, or as shown in Figure 8 of the reaction gas supply nozzle 120 Can bend outward. That is, the central axis of the inert gas supply nozzle 120 at the end of the inert gas supply nozzle 120 may not be parallel to the central axis of the reaction gas supply nozzle 120. As a result, precipitation of silicon at the end of the reaction gas supply nozzle 120 may be prevented.

As shown in FIG. 9, the inert gas supply nozzle 130 may be spaced apart from the reaction gas supply nozzle 120 by a predetermined distance d to inject the inert gas toward the reaction gas supply nozzle 120. In this case, in order to widen the contact surface between the inert gas and the reaction gas supply nozzle 120, the plurality of inert gas supply nozzles 130 may spray the inert gas toward the outer surface of the reaction gas supply nozzle 120.

The reaction gas supply nozzle 120 described above with reference to FIGS. 1, 3, 4, 7, and 9 may supply an etching gas for removing silicon by reacting with silicon along with the reaction gas. In an embodiment of the present invention, the etching gas may include hydrogen chloride. Silicon generates irreversible gasification reactions with hydrogen chloride to produce chlorinated silanes such as trichlorosilane and silane tetrachloride. This gasification reaction occurs instantaneously when the temperature of the reaction tube 110 where the silicon precipitation reaction occurs is 1,000 ° C. Accordingly, the silicon deposited on the reaction gas supply nozzle 120 is gasified and disappeared at a very high speed.

At this time, the reaction gas supply nozzle 120 may supply the reaction gas and the etching gas at the same time or at different times. For example, the reaction gas supply nozzle 120 may supply the reaction gas at the time t1 and then supply the etching gas at the time t2. Alternatively, the reaction gas supply nozzle 120 may supply the reaction gas and the etching gas at the time t1. Even when the reaction gas and the etching gas are supplied at the same time, since the silane chloride is generated by the etching gas, it does not interfere with the production of the polycrystalline silicon product. Accordingly, the operating method of the fluidized bed reactor associated with the reaction gas supply nozzle 120 may be varied depending on the operating conditions or the operating environment.

In the above description, the reaction gas supply nozzle 120 has been described for supplying the etching gas together with the reaction gas, but the inert gas supply nozzle 130 shown in FIGS. 1, 3, 4, 7, and 9 is described. It is also possible to supply the etching gas together with the inert gas. Since the inert gas does not react or weakly reacts with the etching gas, the etching gas may be supplied through the inert gas supply nozzle 130. The inert gas supply nozzle 130 may supply the inert gas and the etching gas at the same time or at different time points.

10 is a plan view of the reaction gas supply nozzle and the inert gas supply nozzle shown in FIGS. 1, 3, 4, and 7. 10 is a plan view taken along the line AA ′ of FIGS. 1, 3, 4, and 7.

Some of the plurality of inert gas supply nozzles 130 may supply an inert gas, and others may supply an etching gas that reacts with silicon to remove silicon. For example, as shown in FIG. 10, an inert gas supply nozzle 130 capable of supplying an etching gas together with an inert gas is positioned above and below the reaction gas supply nozzle 120, and reactant gas supply nozzle 120 is located. Inert gas supply nozzles 130 capable of supplying only inert gas may be positioned on the left and right sides of the reference. At this time, the upper and lower inert gas supply nozzle 130 may supply the inert gas and the etching gas at the same time or may be supplied at different times.

FIG. 11 is another plan view of the reaction gas supply nozzle and the inert gas supply nozzle shown in FIGS. 1, 3, 4, and 7. The reaction gas supply nozzle 120 and the inert gas supply nozzle 130 shown in FIG. 10 are not coaxial with each other, but the reaction gas supply nozzle 120 and the inert gas supply nozzle 130 shown in FIG. 11 are coaxial. At this time, the reaction gas supply nozzle 120 of FIG. 11 is located inside the inert gas supply nozzle 130.

As such, when the reaction gas supply nozzle 120 is not located inside the inert gas supply nozzle 130 but is located outside as shown in FIG. 12, the reaction gas supply nozzle 120 contacts the inert gas supply nozzle 130 ′ as described above with reference to FIG. 5. Since the reaction gas supply nozzle 120 ′ is not cooled, silicon may be deposited on the inner surface of the reaction gas supply nozzle 120 ′.

13 to 17 show other examples of the reaction gas supply nozzles shown in FIGS. 1, 3, 4, 7, 7, and 11.

As shown in FIGS. 13 and 14, the reaction gas supply nozzle 120 may have an injection unit 121 inclined at an angle from a central axis of the reaction gas supply nozzle 120.

That is, as shown in FIG. 13 and FIG. 14, it may have a single injection unit 121 having a center point on the central axis and supplying the reaction gas toward the circumference of the virtual circle perpendicular to the central axis. As the reaction gas is injected in various directions as described above, even if the size of the reaction tube 110 is large, the reaction gas may be quickly and uniformly dispersed in the inner space of the reaction tube 110.

In this case, as shown in FIG. 14, an induction line 123 may be formed on the surface of the injection unit 121 of the reaction gas supply nozzle 120 to guide the outflow direction of the reaction gas. The spiral guide line 123 may have a shape of a protrusion 123a protruding from the surface of the injection part 121 or a shape of a groove 123b recessed in the surface of the injection part 121. The spiral induction line 121 may induce an outflow direction of the reaction gas so that the reaction gas is released in a vortex form. The reaction gas released in the vortex form may be quickly and uniformly dispersed in the inner space of the reaction tube 110 even if the size of the reaction tube 110 is large.

On the other hand, as shown in Figure 15 to 17, the reaction gas supply nozzle 120 may have a plurality of the injection unit 121 for supplying the reaction gas in different directions. Accordingly, even if the size of the reaction tube 110 is large, the reaction gas can be quickly and uniformly dispersed in the inner space of the reaction tube 110.

As described above, since the inert gas supply nozzle 130 surrounds the reaction gas supply nozzle 120, as illustrated in FIGS. 15 to 17, the plurality of injection units 121 may be configured to supply the inert gas supply nozzle 130. Can penetrate

In addition, as illustrated in FIGS. 16 and 17, the reaction gas supply nozzle 120 may further include an injection unit supplying the reaction gas along the central axis of the reaction gas supply nozzle 120. Since the reaction gas supply nozzle 120 further includes an injection unit 125 formed along the central axis in addition to the injection unit 121 having a predetermined angle with the central axis, the reaction gas is more quickly and uniformly distributed in the internal space of the reaction tube 110. Can be.

As shown in FIG. 1, the body 140 of the fluidized bed reactor may include a head 141, a first body 143, a second body 145, and a bottom 147. have.

The head 141 is connected to the first body 143 on the first body 143. In addition, the second body 145 is positioned below the first body 143 and is connected to the first body 143. The bottom portion 147 is positioned below the second body portion 145 and is connected to the second body portion 145.

The body 140 of the fluidized bed reactor according to the embodiment of the present invention includes a head 141, but without a head 141 a plurality of body parts (for example, the first body portion 143 and the second body portion ( 145)) and a bottom portion 147, in which case the upper portion of the first body portion 143 is closed without being opened.

In addition, the body 140 of the fluidized bed reactor according to the embodiment of the present invention may include two or more body parts 143 and 145 but may include two or more body parts.

The inner surface of the head 141 may be made of an inorganic material that is not easily deformed at high temperature. For example, the inner surface of the head 141 may be made of at least one of quartz, silica, silicon nitride, boron nitride, zirconia, silicon carbide, graphite, silicon, and glassy carbon.

In addition, when cooling to the outer surface of the head 141 is possible, at least one of coating (coating) or lining (lining) using the organic polymer on the inner surface of the head 141 may be made.

When the inner surface of the head 141 is made of a carbon-containing material such as silicon carbide, graphite, and glassy carbon, since the polycrystalline silicon may be contaminated by carbon impurities, the inner surface of the head 141 to which the polycrystalline silicon may contact Silver may be coated or lined with materials such as silicon, silica, quartz, silicon nitride, and the like.

For example, unlike the head 141 of FIG. 1, the head 141 of FIG. 18 may include a plurality of partial heads 141a and 141b, and a lining layer may be formed on an inner surface of the first partial head 141a. 141c may be located.

The first body 143 is positioned below the head 141 to be connected to the head 141 and provides an internal space in which the polycrystalline silicon precipitation reaction occurs.

The second body part 145 is positioned below the first body part 143 to be connected to the first body part 143, and together with the first body part 143, at least one of polycrystalline silicon precipitation reaction or heating reaction Provide internal space to rise.

The bottom portion 147 is positioned below the second body portion 145 and is connected to the second body portion 145, and various nozzles 120, 130 and 150, a heater 160, and an electrode for polycrystalline silicon precipitation are provided. 170 and the like are assembled.

When the head 141, the first body 143, and the second body 145 are made of metal, a protective film may be coated on the inner surface thereof, or a protective tube or a protective wall may be additionally installed. The protective layer, the protective layer or the protective layer may be formed of a metal material, but may be coated or lined with a non-metallic material such as an organic polymer, ceramic, quartz, or the like to prevent contamination inside the reactor.

If the size and height of the fluidized bed reactor is increased for mass production of polycrystalline silicon, assembly and installation and maintenance of the fluidized bed reactor may be difficult. That is, when the fluidized bed reactor includes one body portion and a high weighted and heavy body, the reaction tube 110, the handling of the body portion becomes difficult during assembly, installation, and maintenance of the fluidized bed reactor. The pipe 110 may hit and be broken.

On the other hand, the fluidized bed reactor according to the embodiment of the present invention includes a reaction tube 110 including a plurality of body parts 143 and 145, and a first partial reaction tube 110a and a second partial reaction tube 110b. Therefore, the assembly, installation and maintenance of the fluidized bed reactor can be made easily.

The first partial reaction tube 110a and the second partial reaction tube 110b may be in the form of a tube or may include a tube, a cone, and an ellipse portion. Opposing end portions of the first partial reaction tube 110a and the second partial reaction tube 110b may be processed into flanges. The first partial reaction tube 110a and the second partial reaction tube 110b may be formed of a plurality of portions, and some of these portions may be inner wall surfaces of the first body portion 143 and the second body portion 145. It may be installed in the form of a liner (liner).

Since the description of the material of the first partial reaction tube 110a and the second partial reaction tube 110b has been made in the process of describing the material of the reaction tube 110, the description thereof is omitted.

The first partial reaction tube 110a and the second partial reaction tube 110b will be described in more detail later with reference to the drawings.

Next, the assembling process of the fluidized bed reactor according to the embodiment of the present invention will be described in detail.

The first partial reaction tube 110a is assembled to be located inside the first body 143. The second partial reaction tube 110b is assembled to be positioned inside the second body 145, and various nozzles 120 and 130 are provided on the bottom 147 for sealing the lower end of the second body 145. 150, the electrode 170 and the heater 160 are assembled. A bottom portion 147 is connected to a lower portion of the second body portion 145 in which the second partial reaction tube 110b is located. Thereafter, the first body 143 and the second body 145 are connected to each other, and the head 141 is connected to the first body 143.

19A and 19B illustrate a connection structure between a first partial reaction tube and a second partial reaction tube of the fluidized bed reactor of FIGS. 1 and 18.

As shown in FIG. 19A, the first partial reaction tube 110a and the second partial reaction tube 110b are disposed at opposite ends of the first partial reaction tube 110a and the second partial reaction tube 110b, respectively. It includes protrusions (111a, 111b) protruding in the direction of the first body portion 143 and the second body portion (145).

In this case, the protrusion 111a of the first partial reaction tube 110a and the protrusion 111b of the second partial reaction tube 110b may face each other.

Since the contact area between the first partial reaction tube 110a and the second partial reaction tube 110b becomes wider, the risk of breakage when the first partial reaction tube 110a and the second partial reaction tube 110b are connected is reduced.

In addition, as shown in FIG. 19A, in consideration of the durability of the first partial reaction tube 110a and the second partial reaction tube 110b, the support member 113 may include the first partial reaction tube 110a and the second. It is sandwiched between the partial reaction tubes 110b.

The material of the support member 113 may be made of an inorganic material that is not easily deformed at high temperatures, such as quartz, silica, silicon nitride, boron nitride, zirconia, silicon carbide, graphite, silicon, glassy carbon, or a composite of these materials. It may be made of an inorganic material.

When the support member 113 is made of a carbon-containing material such as silicon carbide, graphite, glassy carbon, the carbon-containing material may contaminate the polycrystalline silicon, and thus the surface of the support member 123 to which the polycrystalline silicon may contact may be silicon. Or may be coated or lined with silica, quartz, silicon nitride, or the like.

At this time, the support member 113 can be replaced with a sealing material (not shown), in which case the sealing material (not shown) is sandwiched between the first partial reaction tube 110a and the second partial reaction tube 110b.

Meanwhile, as shown in FIG. 19B, in consideration of the durability of the first partial reaction tube 110a and the second partial reaction tube 110b, the support member 113 may be formed of the first partial reaction tube 110a and the first partial reaction tube 110a. It may be sandwiched between the two-part reaction tube (110b). In addition, as illustrated in FIG. 19B, the sealing member 115 may be sandwiched between the supporting member 113 and the first partial reaction tube 110a and between the supporting member 113 and the second partial reaction tube 110b. .

The sealing material replacing the support member 113 of FIG. 19A or the sealing material 115 of FIG. 19B may have a sheet, knit, or felt shape, which may withstand high temperatures and prevent contamination. It can be made of a fibrous material containing silicon so that. The sealing member 115 replacing the support member 113 of FIG. 19A or the sealing member 115 of FIG. 19B may close a gap between the first partial reaction tube 110a and the second partial reaction tube 110b.

That is, the fluidized bed reactor according to the embodiment of the present invention may include a first partial reaction tube (110a) and a second partial reaction tube (110b) for the convenience of assembly, installation and maintenance, the first partial reaction tube There may be a gap between 110a and the second partial reaction tube 110b. Sealing material replacing the support member 113 of FIG. 19A or the sealing material 115 of FIG. 19B blocks the gap between the first partial reaction tube 110a and the second partial reaction tube 110b so that the silicon particles leak to the outside. Can be prevented.

In addition, the sealing member replacing the support member 113 of FIG. 19A or the sealing member 115 of FIG. 19B may include a first partial reaction tube 110a and a first partial reaction tube 110a and a second partial reaction tube 110b. The risk of breakage of the second partial reaction tube 110b can be reduced.

The various nozzles 150 and 120, the heater 160, the electrode 170, and the like are assembled together with the plates 147a to 147d constituting the bottom portion 147. 5A and 5B, the bottom portion 147 of the fluidized bed reactor according to the embodiment of the present invention includes a base plate 147a and first to third plates 147b, 147c, and 147d. .

The base plate 147a is connected to the second body 145 and the flow gas supply nozzle 150 and the reaction gas supply nozzle 120 are assembled. The base plate 147a may be made of a metal material having excellent mechanical strength and easy processing, such as carbon steel, stainless steel, and other alloy steel.

An insulating material (not shown) may be coated on an area of the base plate 147a that contacts the electrode 170 to insulate the electrode 170 and the base plate 147a from each other. The electrode 170 may be made of graphite, silicon carbide, a metal material, or a composite thereof. The shape of the electrode 170 may be a cable, a rod, a rod, a molding, an outlet, a coupler, a bar, a braided wire, or a combination thereof.

In addition to such an insulation method, an electrode 170 coated with an insulation material may be inserted into the base plate 147a. The insulation method between the base plate 147a and the electrode 170 is not limited to the insulation method mentioned above, and various insulation methods may be applied to the fluidized bed reactor according to the embodiment of the present invention.

The first plate 147b is positioned on the base plate 147a to insulate the base plate 147a. Accordingly, the first plate 147b may be made of a material such as quartz that does not contaminate the deposited polycrystalline silicon while having insulation. The first plate 147b may be made of a ceramic material having heat resistance at a high temperature such as silicon nitride, alumina, yttria, etc., in addition to quartz. In some cases, the first plate 147b may be formed on the surface of the first plate 147b with such a ceramic material. It may be coated or lined.

The second plate 147c is positioned on the first plate 147b and contacts the electrode 170 and the heater 160 to supply electricity to the heater 160. The second plate 147c may be made of a conductive material such as graphite, graphite coated with silicon carbide, silicon carbide, and graphite coated with silicon nitride.

Since the first plate 147b having an insulating property is positioned between the base plate 147a and the second plate 147c, the base plate 147a and the second plate 147c are insulated from each other.

Since the second plate 147c is in contact with the heater 160, heat may be generated in the second plate 147c, but the second plate 147c may have a larger cross-sectional area through which current flows in the second plate 147c than the heater 160. The heat generated at 147c is very small compared to the heat generated at the heater 160. In addition, a graphite sheet having excellent ductility may be inserted between the second plate 147c and the heater 160 to reduce heat generated in the second plate 147c.

When the base plate 147a and the second plate 147c are conductive, leakage current flowing to the base plate 147a may occur due to the contact between the base plate 147a and the second plate 147c. Accordingly, as shown in FIGS. 1 and 18, the ends of the base plate 147a and the second plate 147c may be spaced apart by a predetermined distance d. A groove in which the second plate 147c may be seated may be formed in the first plate 147b so as to be spaced apart by a predetermined distance d. For example, the first plate 147b may have a groove equal to or greater than the length of the second plate 147c so that the second plate 147c may be seated in the groove of the first plate 147b. Accordingly, since a part of the first plate 147b may be located between the ends of the base plate 147a and the second plate 147c, insulation between the base plate 147a and the second plate 147c may be maintained. have.

As shown in FIG. 1, the base plate 147a and the second plate 147c may be insulated by the first plate 147b, and wrap around the second plate 147c as shown in FIG. 18. By installing the insulating ring 300, the base plate 147a and the second plate 147c may be insulated. At this time, the insulating ring 300 may be made of quartz, ceramic.

The third plate 147d is disposed on the second plate 147c so that the polycrystalline silicon precipitated inside the first partial reaction tube 110a and the second partial reaction tube 110b is contaminated by the second plate 147c. It is prevented from becoming and has an insulation function.

The third plate 147d may be made of an inorganic material that is not easily deformed at high temperature, and may be made of quartz, silica, silicon nitride, boron nitride, zirconia, silicon carbide, graphite, silicon, glassy carbon, or a composite thereof. Can be.

When the third plate 147d is made of a carbon-containing material such as silicon carbide, graphite, and glassy carbon, the carbon-containing material may contaminate the polycrystalline silicon. Thus, the surface of the third plate 147d may be silicon, silica, quartz, Coating or lining with silicon nitride or the like.

FIG. 20 illustrates an assembly structure of plates and a heater of the fluidized bed reactor of FIGS. 1 and 18. As shown in FIG. 20, the base plate 147a by the fixing bolt 800 penetrating through the base plate 147a, the first plate 147b, the second plate 147c, and the third plate 147d, The first plate 147b, the second plate 147c, and the third plate 147d may be fixed.

As illustrated in FIG. 20, the plurality of plates 147a to 147d included in the bottom portion 147 may be fixed by the fixing bolt 800 through the plurality of plates 147a to 147d.

The fixing bolt 800 may be made of an inorganic material that is not easily deformed at high temperature in order to prevent contamination of polycrystalline silicon formed in the first partial reaction tube 110a and the second partial reaction tube 110b. It may be made of an inorganic material such as quartz, silica, silicon nitride, boron nitride, zirconia, silicon, or a composite of these materials.

When the fixing bolt 800 is made of a carbon-containing material such as silicon carbide, graphite, glassy carbon, the surface of the fixing bolt 800 is silicon, silica, quartz, silicon nitride, etc. to prevent contamination of polycrystalline silicon due to the carbon-containing material. Can be coated or lined with a cap made of silicon, silica, quartz, silicon nitride, or covered with a fixing bolt 800. The fixing bolt 800 is screwed with the plurality of plates 147a to 147d.

Meanwhile, a fixing part 810 inserted into the heater 160 is installed in the first plate 147b of the bottom part 147 to which the heater 160 is assembled. The fixing part 810 such as a pin or a clip is inserted into a perforation formed in the second plate 147c connected to the heater 160 among the plates 147a, 147b, 147c, and 147d of the bottom part 250.

The heater 160 has grooves g1 and g2 into which the fixing part 810 is inserted, and a manufacturer or a user presses the heater 160 into the fixing part 810 so that the heater 160 is inserted into the bottom part 147. Can be fixed at Therefore, since assembly of the heater 160 does not require fastening of screws and bolts, the assembly of the heater 160 may be easily performed.

In this embodiment, since the heater 160 has a U shape, two fixing parts 810 are required for each heater 160, but the number of fixing parts 810 may vary according to the shape of the heater 160. have. The fixing part 810 may be made of a material having excellent electrical conductivity and ductility, such as graphite or metal material.

The second plate 147c includes a plurality of unit plates 147c-1 and 147c-2, and the lower portion of the heater 160 contacts the unit plates 147c-1 and 147c-2 adjacent to each other. Electricity is supplied through the unit plates 147c-1 and 147c-2 of the two plate 147c.

In this case, the heater 160 includes a protrusion 160a extending from the bottom of the heater 160 in a direction perpendicular to the length direction of the heater 160. The protrusion 160a of the heater 160 may have grooves g1 and g2, and the fixing portion 810 is inserted into the grooves g1 and g2 of the protrusion 160a, and at the same time, the protrusion 160a is formed as a third. Since it is covered by the plate 147d, the fixing of the heater 160 may be made more stable.

Adjacent unit plates 147c-1 and 147c-2 are insulated from each other. For example, an insulator 163 may be located between the unit plates 147c-1 and 147c-2 of the second plate 147c in contact with the lower portion of the heater 160. The insulator 163 insulates between the unit plates 147c-1 and 147c-2 contacting the lower portion of the heater 160 to prevent the occurrence of leakage current.

In an embodiment of the present invention, wrinkles may be formed on the surface of the heater 160, thereby increasing the surface area per unit volume of the heater 160 to increase heating efficiency. The increase in the surface area per unit volume of the heater 160 may be formed with protrusions or patterns of various shapes protruding from the surface of the heater 160 in addition to wrinkles, but is not limited thereto.

After the fixing part 810 is inserted into the heater 160, a heater cap 161 is provided to the heater 160 to protect the heater 160 and to prevent contamination of the polycrystalline silicon by the heater 160. The outer surface of the heater 160 is not exposed to the inner space 111.

In order to perform the role of the heater cap 161, the heater cap 161 may be made of an inorganic material that is not easily deformed at high temperature, and may include quartz, silica, silicon nitride, boron nitride, zirconia, yttria, silicon, or the like. It may be made of an inorganic material such as a composite in which the materials are mixed.

When the heater cap 161 is made of carbon-containing materials such as silicon carbide, graphite, and glassy carbon, the surface of the heater cap 161 may be silicon, silica, quartz, silicon nitride, or the like to prevent contamination of polycrystalline silicon due to the carbon-containing material. It can be coated or lined with.

The heater cap 161 includes a locking jaw 161a extending in a direction perpendicular to the longitudinal direction of the heater cap 161, and the locking jaw 161a of the heater cap 161 is formed of the third plate 147d. The plurality of unit plates 147d-1 and 147d-2 are sandwiched and fixed.

It will be apparent to those skilled in the art that the present invention can be embodied in other specific forms without departing from the spirit or scope of the invention as defined in the appended claims. It is obvious to them. Therefore, the above-described embodiments should be regarded as illustrative rather than restrictive, and thus, the present invention is not limited to the above description and may be modified within the scope of the appended claims and their equivalents.

Claims (22)

A reaction tube in which precipitation of silicon occurs;
A reaction gas supply nozzle for supplying a reaction gas capable of causing precipitation of the silicon to an inner space of the reaction tube; And
At least one inert gas supply nozzle for supplying the silicon and the inert gas which is inert to cool part or all of the reaction gas supply nozzle located in the internal space,
The reaction gas supply nozzle supplies an etching gas that reacts with the silicon to remove the silicon together with the reaction gas,
The reaction gas supply nozzle has an injection portion inclined from the central axis of the reaction gas supply nozzle,
A plurality of the injection portion is a fluidized bed reactor, characterized in that through the inert gas supply nozzle. The method of claim 1,
The inert gas supply nozzle is in contact with a part or all of the outer surface of the reaction gas supply nozzle surrounding the part or all of the outer surface of the reaction gas supply nozzle. 3. The method of claim 2,
The height of the inert gas supply nozzle is a fluidized bed reactor, characterized in that equal to or greater than the height of the reaction gas supply nozzle. The method of claim 3,
And a central axis of the inert gas supply nozzle at an end of the inert gas supply nozzle crosses a central axis of the reaction gas supply nozzle. The method of claim 1,
And the inert gas supply nozzle is spaced apart from the reaction gas supply nozzle to inject the inert gas toward the reaction gas supply nozzle. delete The method of claim 1,
The reaction gas supply nozzle is a fluidized bed reactor, characterized in that for supplying the reaction gas and the etching gas at the same time or at different times. The method of claim 1,
The inert gas supply nozzle is a fluidized bed reactor, characterized in that for supplying the etching gas with the inert gas to react with the silicon to remove the silicon. 9. The method of claim 8,
The inert gas supply nozzle supplies the inert gas and the etching gas at the same time or at different times. The method of claim 1,
A part of the plurality of inert gas supply nozzles supplies the inert gas, and the other supplies an etching gas that reacts with the silicon to remove the silicon along with the inert gas. The method of claim 1,
The reaction gas supply nozzle and the inert gas supply nozzle are coaxial, and the reaction gas supply nozzle is located inside the inert gas supply nozzle. delete The method of claim 1,
The reaction gas supply nozzle
And one injection section having a center point on the central axis and supplying the reaction gas toward a circumference of a virtual circle perpendicular to the central axis. The method of claim 1,
Fluidized bed reactor, characterized in that the spiral induction line is formed on the surface of the injection portion of the reaction gas supply nozzle to guide the outflow direction of the reaction gas. 15. The method of claim 14,
The reaction gas is a fluidized bed reactor characterized in that the discharge direction is guided by the spiral induction line is discharged in the form of vortex. The method of claim 1,
The reaction gas supply nozzle has a plurality of the injection unit for supplying the reaction gas in different directions. delete 17. The method of claim 16,
The reaction gas supply nozzle further comprises a spraying unit for supplying the reaction gas along the central axis of the reaction gas supply nozzle. The method according to any one of claims 1 to 5, 7 to 11, 13 to 16, and 18,
The inert gas includes a hydrogen, an inert gas, or a mixed gas of the hydrogen and the inert gas. The method according to any one of claims 1 to 5, 7 to 11, 13 to 16, and 18,
Fluidized bed reactor characterized in that the temperature of the inert gas is lower than the temperature of the internal space. The method according to any one of claims 1 to 5, 7 to 11, 13 to 16, and 18,
The fluidized bed reactor further includes a body in which the reaction tube is installed therein,
The body includes a first body portion, a second body portion and a bottom portion,
The second body portion is located below the first body portion is connected to the first body portion,
The bottom portion is located below the second body portion is connected to the second body portion, fluidized bed reactor, characterized in that the reaction gas supply nozzle and the inert gas supply nozzle is installed. The method according to any one of claims 1 to 5, 7 to 11, 13 to 16, and 18,
The fluidized bed reactor further includes a body in which the reaction tube is installed therein,
The body includes a first body portion, a second body portion and a bottom portion,
The bottom portion
A base plate connected to the second body and provided with the reaction gas supply nozzle and the inert gas supply nozzle;
A first plate positioned on the base plate to insulate the base plate,
A second plate positioned on the first plate and contacting the heater for supplying heat to the internal space to supply electricity to the heater;
And a third plate having an insulating function to prevent the polycrystalline silicon deposited on the second plate from being contaminated by the second plate and having an insulating function.

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