KR20130138033A - Siemens reactor comprising plasma generator and method for manufacturing polysilicon using the same - Google Patents

Siemens reactor comprising plasma generator and method for manufacturing polysilicon using the same Download PDF

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Publication number
KR20130138033A
KR20130138033A KR1020120061813A KR20120061813A KR20130138033A KR 20130138033 A KR20130138033 A KR 20130138033A KR 1020120061813 A KR1020120061813 A KR 1020120061813A KR 20120061813 A KR20120061813 A KR 20120061813A KR 20130138033 A KR20130138033 A KR 20130138033A
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South Korea
Prior art keywords
reaction
gas
plasma
plasma generator
polysilicon
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KR1020120061813A
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Korean (ko)
Inventor
이정우
류창석
이동철
김균중
최광욱
유진형
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주식회사 엘지화학
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Priority to KR1020120061813A priority Critical patent/KR20130138033A/en
Publication of KR20130138033A publication Critical patent/KR20130138033A/en

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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
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/087—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
    • 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
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0894—Processes carried out in the presence of a plasma

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Silicon Compounds (AREA)

Abstract

The present invention relates to a Siemens reaction apparatus including a reaction chamber, a gas supply part and a silicon rod, and to a Siemens reaction apparatus including a plasma generator in the reaction chamber and a polysilicon manufacturing method using the same.

Description

SIEMENS REACTOR COMPRISING PLASMA GENERATOR AND METHOD FOR MANUFACTURING POLYSILICON USING THE SAME

The present invention relates to a Siemens reactor for producing polysilicon, and more particularly, by installing a plasma generator inside the Siemens reactor, the reaction can be performed at atmospheric pressure, and the energy can be reduced by increasing the dissociation rate of the reaction gas. A Siemens reactor.

Polysilicon is a material that is used as a raw material for semiconductor devices and solar cell devices, and its demand is gradually increasing. Such polysilicon may be prepared by reacting trichlorosilane gas with hydrogen gas, as shown in Scheme 1 below.

[Reaction Scheme 1]

SiHCl 3 + H 2 → Si + 3HCl

Currently, commercially available high purity polysilicon is mostly manufactured by chemical vapor deposition method called Siemens process. Polysilicon production apparatus according to the conventional Siemens method is provided with a silicon rod inside the vertical reactor, the end of the silicon rod is connected to the electrode. In addition, a gas supply nozzle is provided for supplying trichlorosilane gas and hydrogen gas, which are reaction gases, into the reactor.

The method of forming polysilicon using the conventional Siemens reactor configured as described above is as follows. First, current flows through the electrode to the silicon rod, and the reaction gas is supplied into the reactor through the gas supply nozzle. The silicon rod is heated to a surface temperature of about 1000 to 1150 ° C. by the supplied electric power, and a high purity polysilicon is deposited on the silicon rod as the reaction gas is pyrolyzed on the heated silicon rod surface.

However, such a conventional Siemens reactor typically consumes a lot of electrical energy of about 65 ~ 200KWh / kg, the cost of this electrical energy is a very large proportion of the polysilicon manufacturing cost. Therefore, in order to lower the polysilicon manufacturing cost, it is necessary to develop a technology capable of producing polysilicon with little energy.

The present invention is to solve the above problems, it is possible to produce a polysilicon even at atmospheric pressure by installing a plasma generator in the gas supply nozzle inside the Siemens reaction apparatus, increase the dissociation rate of the reaction gas is required for the polysilicon production reaction It is to provide a Siemens reaction apparatus and a polysilicon manufacturing method using the same that can increase energy efficiency by reducing energy consumption.

The object of the present invention is not limited to the above description. The problem of the present invention will be understood from the general contents of the present specification, those skilled in the art will have no difficulty understanding the additional problem of the present invention.

In order to solve the above problems, the present invention provides a Siemens reaction apparatus including a plasma generator in the gas supply unit inside the reaction chamber in the Siemens reaction apparatus including a reaction chamber, a gas supply unit and a silicon rod.

In this case, the plasma generator, an arc discharge method, an RF plasma torch method, a corona discharge method, an atmospheric pressure plasma jet method, a microwave induced plasma u -wave induced plasma) may be any one of the methods, but is not limited thereto.

On the other hand, the gas supply unit preferably comprises a nozzle for supplying gas to the reaction chamber, the plasma generator is preferably located at the end of the nozzle.

In addition, the nozzle is preferably located between the silicon rod and the gas supply.

On the other hand, when producing polysilicon using the Siemens reactor, the pressure inside the reaction chamber is preferably atmospheric pressure.

On the other hand, using the plasma generator provides a Siemens reaction apparatus for decomposing the reaction gas trichlorosilane (TCS) and hydrogen (H 2 ) gas mixture into a plasma state.

Meanwhile, in the Siemens reaction apparatus including the reaction chamber, the gas supply part, and the silicon rod of the present invention, supplying a reaction gas into the reaction chamber through a gas supply part, plasma treating the reaction gas, and the reaction gas is silicon. It provides a polysilicon manufacturing method comprising the step of depositing on the rod to form polysilicon.

At this time, the reaction gas is preferably gas trichlorosilane (TCS) and hydrogen (H 2 ) gas mixture.

In addition, the forming of the polysilicon, preferably, the temperature of the silicon rod is performed at 300 to 800 ℃, but is not limited thereto.

On the other hand, the present invention provides a polysilicon production method using the Siemens reactor.

In addition, the solution of the above-mentioned problems does not list all the features of the present invention. The various features of the present invention and the advantages and effects thereof will be more fully understood by reference to the following specific embodiments.

According to the present invention, a gas supply unit including a plasma generator is installed inside the Siemens reactor, so that polysilicon can be produced even at atmospheric pressure, and the energy required for the polysilicon production reaction can be maximized by increasing the dissociation rate of the reaction gas. Has the characteristics.

1 is a schematic view showing the structure of a Siemens reaction apparatus according to an embodiment of the present invention.
2 is a schematic view showing the structure of an arc discharge plasma generator according to an embodiment of the present invention.
Figure 3 is a schematic diagram showing the structure of the RF plasma torch plasma generator according to an embodiment of the present invention.
4 is a schematic view showing the structure of a corona discharge plasma generator according to an embodiment of the present invention.
5 is a schematic view showing the structure of an atmospheric plasma jet plasma generator according to an embodiment of the present invention.
6 is a schematic view showing the structure of a microwave induced plasma generator according to an embodiment of the present invention.

Hereinafter, the present invention will be described more specifically with reference to the drawings. However, the following drawings are intended to facilitate the understanding of the present invention, and are merely examples of the present invention, and the scope of the present invention is not limited to the ranges described in the drawings. In addition, the following drawings may be represented by some components are exaggerated, reduced or omitted for a smooth understanding of the invention.

The inventors of the present invention have repeatedly studied to reduce the energy of the Siemens reaction apparatus used in the polysilicon manufacturing method, and as a result, by including the plasma generator in the gas supply of the Siemens reaction apparatus, the above object can be achieved. The present invention was completed.

1 is a perspective view of a Siemens reactor including a plasma reactor, which is an embodiment of the present invention. As shown in FIG. 1, the Siemens reactor of the present invention includes a reaction chamber 50, a gas supply unit 20, and a silicon rod 30, wherein a plasma is supplied to a gas supply unit of the reaction chamber. The generator 10 is included.

As in the present invention, when the plasma generator is installed in the gas supply unit inside the Siemens reactor, the dissociation rate of the reaction gas required for the reaction may be increased to reduce energy required for the surface precipitation process of the polysilicon. Therefore, polysilicon may be produced at a lower temperature than the conventional Siemens process, and polysilicon production may be performed even at atmospheric pressure. In addition, there is an effect that can increase the energy efficiency by lowering the thermal energy required for the reaction.

The plasma generator 10 may include an arc discharge method, an RF plasma torch method, a corona discharge method, an atmospheric pressure plasma jet method, and a microwave induction method. Preferably, any one of a plasma (u-wave induced plasma) method is not limited thereto.

On the other hand, Figure 2 is a schematic diagram of an arc discharge plasma generator, according to an embodiment of the present invention. As shown in FIG. 2, the reaction gas is discharged in a plasma state while passing through the space 3 between the cathode electrode 1 and the anode electrode 2. At this time, the coolant passes through the inside 4 of the anode electrode 2 and serves to lower the temperature of the plasma generator.

In addition, the arc discharge plasma generator is not limited to this, but using a direct current power source, using an applied voltage of several tens of volts (V), there is an advantage that can obtain a high conductivity and ultra-high density plasma.

On the other hand, Figure 3 is a schematic diagram of an RF plasma torch plasma generator, according to an embodiment of the present invention. As shown in FIG. 3, the reaction gas is discharged into the plasma state by the induction coil 5 while passing through the interior 6 of the plasma generator. At this time, while the coolant passes through the outer side 7 of the induction coil serves to lower the temperature of the plasma generator.

In addition, the RF plasma torch plasma generator, but not limited to this, by using an RF AC power source having a frequency of several MHz, using a voltage of about 100 volts (V), to prevent damage to the wall of the equipment and contamination of the product There is an advantage that can be prevented.

On the other hand, Figure 4 is a schematic diagram of a corona discharge plasma generator, according to an embodiment of the present invention. As shown in FIG. 4, the corona discharge plasma generator includes a first ground electrode 11 having a plurality of precipitation electrodes on which a high voltage electrode is formed, and a flat plate formed on opposing surfaces of the first ground electrode 11. The second ground electrode 12 is a type ground electrode, and the reaction gas is discharged in a plasma state while passing between the first ground electrode 11 and the second ground electrode 12.

In addition, the corona discharge plasma generator is not limited to this, but using a direct current power source, using an applied voltage of several tens of volts (V), there is a feature that can discharge a large area.

On the other hand, Figure 5 is a schematic diagram of an atmospheric plasma jet plasma generator, according to an embodiment of the present invention. As shown in FIG. 5, the atmospheric plasma jet plasma generator includes a cylindrical cathode electrode 21, a cathode electrode 22 having a shape in which a predetermined distance from the cathode electrode is rotated while wrapping the cathode electrode in a cone shape, and the It consists of a coolant inlet 24 and a gas inlet 23 located at the lower end of the anode electrode. At this time, the reaction gas is introduced into the plasma generator through the gas inlet 23 and discharged in the plasma state.

On the other hand, the atmospheric plasma jet plasma generator is not limited to this, it is characterized by using an AC power source, using a voltage of about 100 volts (V).

6 shows a schematic diagram of a microwave induced plasma generator, in accordance with an embodiment of the present invention. As shown in FIG. 6, the microwave induced plasma generator is composed of a microwave generator 31, a waveguide 32, a three-stage tuner 33, and a plasma generator 34.

At this time, the microwave generated by the microwave generator 31 is supplied to the plasma generator 34 via the waveguide 32 to discharge the reaction gas in the plasma state. On the other hand, the three-stage tuner 33 serves to increase the output efficiency by minimizing the reflection by matching the impedance generated between the waveguide and the plasma generator.

In addition, the microwave-induced plasma generator is not limited thereto, but uses a microwave (u-wave) as a power source, and requires a precisely designed microwave antenna (u-wave antenna).

On the other hand, the gas supply unit 20 includes a nozzle for supplying gas to the reaction chamber, but is not limited to this, it is preferable that the plasma generator is located at the end of the nozzle.

In addition, the nozzle is preferably located between the silicon rod 30 and the gas supply unit 20, but is not limited thereto.

Meanwhile, a mixture of trichlorosilane (TCS) and hydrogen (H 2 ) gas, which are reaction gases, is introduced into the reactor through a gas supply unit including the nozzle, and the reaction gas passing through the nozzle is dissociated by a plasma generator to release silicon rods. It is supplied to the surface of. In this case, the dissociation rate of the reaction gas has a dissociation rate of about 2 to 3 times higher than that of a general Siemens reactor, and the reaction gas having a high dissociation rate is precipitated in the process of being adsorbed and diffused on the surface of the silicon rod. Will produce polysilicon.

In addition, the reaction gas introduced into the reactor through the nozzle of the gas supply unit including the plasma generator is adsorbed onto the surface of the silicon rod, and the larger the area where the reaction gas is in contact with the silicon rod, the more polysilicon is deposited. .

Therefore, when the silicon rod is disposed in a form surrounding the nozzle of the gas supply unit, the area where the reaction gas and the silicon rod contact each other becomes wider, so that the amount of precipitation of polysilicon increases.

On the other hand, the pressure inside the reaction chamber during the production of polysilicon using the Siemens reaction device is preferably atmospheric pressure. The pressure of the reactor due to the feed gas is mutually exclusive in terms of increasing production and maintaining plasma discharge, but atmospheric pressure is an ideal condition that satisfies both conditions. That is, when the pressure inside the chamber is at atmospheric pressure, the production can be increased while maintaining the plasma discharge.

On the other hand, in the Siemens reaction apparatus of the present invention, it is preferable to decompose a trichlorosilane (TCS) and hydrogen (H 2 ) gas mixture which is a reaction gas into a plasma state using the plasma generator.

In addition, the polysilicon is formed, the temperature of the silicon rod may be performed at 300 to 800 ℃, or 450 to 750 ℃.

At this time, the trichlorosilane (TCS) and hydrogen (H 2 ) gas mixture is decomposed into a plasma state by the plasma generator while being supplied into the reaction reaction chamber through a gas supply, the silicon rod is a surface temperature by the supplied power Is heated to 300 to 800, or 450 to 750 ° C., the mixture in the plasma state is pyrolyzed at the silicon rod surface. Then, polysilicon of high purity is deposited on the silicon rod through a reaction as in Scheme 1 below.

[Reaction Scheme 1]

SiHCl 3 + H 2 → Si + 3HCl

More specifically, when the temperature range of the silicon rod is 300 to 500 ℃, it is advantageous for the high-density single crystal growth of polysilicon, the growth rate when 500 to 800 ℃, and the density of the final product at 400 to 600 ℃ It is suitable for the mutual harmony of growth rate. At this time, the temperature setting of each polysilicon generation process may be set by the dissociation rate variation according to the power and frequency control of the plasma.

In the case of polysilicon production reaction as in Scheme 1, energy more than activation energy is required for the reaction to proceed. However, in the case of the present invention, since the plasma generator is installed inside the reaction chamber, and the reaction gas trichlorosilane and hydrogen gas mixture is prepared in a plasma state, the dissociation rate of the reaction gas is increased by two to three times. Therefore, less energy is required for the reaction.

In addition, the conventional Siemens reaction apparatus had to raise the surface temperature of the silicon rod to about 1100 ° C. for the polysilicon production reaction, but when the plasma generator was included in the reaction chamber, the ratio of the reaction gas was higher than that of the conventional Siemens reaction apparatus. Since the rate of dissociation by the plasma generator increases two to three times, the reaction can be performed only at a temperature of about 450 ° C to 750 ° C, and the power consumption required for polysilicon production can be saved, and productivity and cost can be reduced. It works.

In other words, the reaction gas of trichlorosilane and hydrogen gas, which is a reaction gas, has a higher rate of dissociation by a plasma generator, consumes less energy for ionization, and the reaction proceeds with less energy than a conventional polysilicon reaction. Therefore, the surface temperature of the silicon rod can be set lower than that of the conventional method, so that less current can be applied to the silicon rod, thereby saving energy.

Likewise, the surface temperature of the silicon rod is set lower than that of the conventional method, and the energy consumption is reduced by turning the cooler to control the internal temperature rise.

On the other hand, the Siemens reactor of the present invention includes a gas discharge portion 40, by allowing the unreacted gas and the carrier gas to be discharged to the outside of the reaction chamber 50, to prevent the pressure inside the rise.

On the other hand, the polysilicon manufacturing method according to the present invention, supplying a reaction gas into the reaction chamber 50 through the gas supply unit 20, the step of plasma processing the reaction gas, and the reaction gas is a silicon rod ( 30) to form polysilicon.

The present invention also provides a method for producing polysilicon using the Siemens reactor.

10: plasma generator
20: gas supply part
30: silicon rod
40: gas outlet
50: reaction chamber
1: Cathode electrode of arc discharge plasma generator
2: anode of arc discharge plasma generator
5: Induction coil of RF plasma torch plasma generator
11: first ground electrode of corona discharge plasma generator
12: second ground electrode of the corona discharge plasma generator
21: Cathode electrode of atmospheric plasma jet plasma generator
22: anode of atmospheric plasma jet plasma generator
23: gas inlet of atmospheric plasma jet plasma generator
24: Cooling water inlet of the atmospheric plasma jet plasma generator
31: microwave generator of the microwave induction plasma generator
32: Waveguide of the microwave induced plasma generator
33: Three stage tuner of microwave induction plasma generator
34: plasma generator of the microwave induced plasma generator

Claims (10)

In the Siemens reactor comprising a reaction chamber, a gas supply and a silicon rod,
Siemens reactor comprising a plasma generator in the gas supply inside the reaction chamber.
The method of claim 1,
The plasma generator is an arc discharge method, an RF plasma torch method, a corona discharge method, an atmospheric pressure plasma jet method, a microwave induced plasma (u-wave). Siemens reaction system of any one of the induced plasma) method.
The method of claim 1,
The gas supply unit includes a nozzle for supplying gas to the reaction chamber,
Siemens reaction device wherein the plasma generator is located at the end of the nozzle.
The method of claim 3, wherein
The nozzle is a Siemens reactor is located between the silicon rod and the gas supply.
The method of claim 1,
Siemens reactor of the pressure inside the reaction chamber in the production of polysilicon.
The method of claim 1,
Siemens reactor for decomposing the reaction gas trichlorosilane (TCS) and hydrogen (H 2 ) gas mixture to a plasma state using the plasma generator.
In the Siemens reactor comprising a reaction chamber, a gas supply and a silicon rod,
Supplying a reaction gas into the reaction chamber through a gas supply;
Plasma treating the reaction gas; And
Polysilicon is formed by depositing the reaction gas on a silicon rod.
8. The method of claim 7,
The reaction gas is a polysilicon production method of trichlorosilane (TCS) and hydrogen (H 2 ) gas mixture.
8. The method of claim 7,
The polysilicon forming step, the temperature of the silicon rod is polysilicon manufacturing method performed at 300 to 800 ℃.
A method for producing polysilicon using the Siemens reactor of any one of claims 1 to 6.
KR1020120061813A 2012-06-08 2012-06-08 Siemens reactor comprising plasma generator and method for manufacturing polysilicon using the same KR20130138033A (en)

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KR1020120061813A KR20130138033A (en) 2012-06-08 2012-06-08 Siemens reactor comprising plasma generator and method for manufacturing polysilicon using the same

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