Method and apparatus for preparation of granular polysilicon
IPC분류정보
국가/구분
United States(US) Patent
등록
국제특허분류(IPC7판)
C01B-033/021
B01J-008/24
출원번호
US-0609414
(2009-10-30)
등록번호
US-8821827
(2014-09-02)
우선권정보
KR-10-2006-0075897 (2006-08-10)
발명자
/ 주소
Kim, Hee Young
Yoon, Kyung Koo
Park, Yong Ki
Choi, Won Choon
출원인 / 주소
Korea Research Institute of Chemical Technology
대리인 / 주소
Frommer Lawrence & Haug LLP
인용정보
피인용 횟수 :
0인용 특허 :
13
초록▼
An apparatus for preparing granular polysilicon comprises a reactor tube, a reactor shell, an internal heater, and components for controlling pressure, supplying a fluidizing gas and a reaction gas, discharging gas, and discharging particles. The reactor tube is associated with an inner space compri
An apparatus for preparing granular polysilicon comprises a reactor tube, a reactor shell, an internal heater, and components for controlling pressure, supplying a fluidizing gas and a reaction gas, discharging gas, and discharging particles. The reactor tube is associated with an inner space comprising an inner zone that contains a bed of silicon particles and is the site at which silicon deposition occurs. The inner zone comprises a heating zone and a reaction zone. The fluidizing gas supplying component supplies a fluidizing gas for fluidizing the bed of silicon particles to a bottom of the heating zone. The apparatus can minimize the problems occurring during the heating of silicon particles at high temperature for silicon deposition on the surface of the silicon particles.
대표청구항▼
1. An apparatus for preparing granular polysilicon comprises: a reactor tube, an inner space of which comprises a heating zone and a reaction zone above the heating zone, wherein the inner space comprises an inner zone where the bed of silicon particles is present and silicon deposition occurs;a rea
1. An apparatus for preparing granular polysilicon comprises: a reactor tube, an inner space of which comprises a heating zone and a reaction zone above the heating zone, wherein the inner space comprises an inner zone where the bed of silicon particles is present and silicon deposition occurs;a reactor shell enclosing the reactor tube, wherein a space in between the reactor tube and the reactor shell comprises an outer zone where the bed of silicon particles is not present and silicon deposition does not occur;an inert gas connecting means that maintains a substantially inert gas atmosphere in the outer zone;a pressure controlling means that measures and/or controls an inner zone pressure (Pi) and/or an outer zone pressure (Po), and a pressure-difference controlling means that maintains the difference in the outer zone pressure (Po) and the inner zone pressure (Pi) in the range of about 0.01 bar to about 1 bar;a fluidizing gas supplying means that supplies a fluidizing gas for fluidizing the bed of silicon particles to a bottom of the heating zone, and comprises a gas distribution means for distributing the fluidizing gas across the cross-section at the bottom of the heating zone, wherein the gas distribution means comprises a gas distribution plate or a gas distribution assembly having a plurality of holes and/or nozzles that are arranged to distribute the fluidizing gas across the cross-section at the bottom of the heating zone;a reaction gas supplying means installed within the bed of silicon particles and supplying a reaction gas required for silicon deposition into the bed of silicon particles;an internal heater installed in a space in between the reaction gas supplying means and the inner wall of the reactor tube, wherein the internal heater and the reaction gas supplying means are installed vertically from the gas distribution means through the cross-section at the bottom of the heating zone, the internal heater and the reaction gas supplying means intersecting with the gas distribution means, such that the gas distribution plate or the gas distribution assembly surrounds the intersection of the internal heater with the gas distribution means, and surrounds the intersection of the reaction gas supplying means with the gas distribution means;a gas discharging means discharging an off-gas out of the reactor shell; anda particle discharging means discharging a part of the silicon particles prepared in the reactor tube, wherein the height of the reaction gas outlet is located higher than the fluidizing gas outlets, is selected as the reference height for dividing the reaction zone and the heating zone, and the height of the internal heater is higher than the fluidizing gas outlets, but not higher than the reaction gas outlet, for heating the fluidizing gas and the silicon particles in the heating zone. 2. The apparatus for preparing granular polysilicon as set forth in claim 1, wherein the form of the gas distribution plate is selected from a grid, a disc or a conical plate. 3. The apparatus for preparing granular polysilicon as set forth in claim 1, wherein a packed bed of packing materials is formed in a space, which is formed in the heating zone and enclosed by the inner wall of the reactor tube, the fluidizing gas supplying means, the reaction gas supplying means and the internal heater, using packing materials that are not fluidized by the flow of the fluidizing gas. 4. The apparatus for preparing granular polysilicon as set forth in claim 3, wherein silicon product particles are discharged through the particle discharging means after residing in or moving through a space formed between the packing materials. 5. The apparatus for preparing granular polysilicon as set forth in claim 3, wherein the packing materials have an average diameter of 5-50 mm and have a shape selected from the group consisting of sphere, bead, ball, granule, fragment, lump, spheroid, polyhedron, pebble, pellet, ring, nugget, and a mixture thereof. 6. The apparatus for preparing granular polysilicon as set forth in claim 3 or claim 5, wherein the packing materials are made of a material selected from the group consisting of quartz, silica, silicon nitride, boron nitride, silicon carbide, graphite, silicon, glassy carbon, and a mixture thereof. 7. The apparatus for preparing granular polysilicon as set forth in claim 6, wherein the packing materials consist of a single component material or of a plurality of layers in the thickness direction, each layer of which is made of a different material. 8. The apparatus for preparing granular polysilicon as set forth in claim 1, wherein an insulating material is equipped at the outer zone. 9. The apparatus for preparing granular polysilicon as set forth in claim 1, further comprises a supplemental heater installed in the outer zone. 10. The apparatus for preparing granular polysilicon as set forth in claim 9, wherein a heat load of the supplemental heater is within the range of 10-100% of a heat load of the internal heater. 11. The apparatus for preparing granular polysilicon as set forth in claim 1, further comprises a waveguide, which transmits the microwave generated by a microwave generator, or a microwave generator, wherein the waveguide or the microwave generator is coupled with the reactor shell to supply the microwave into the inner zone. 12. The apparatus for preparing granular poly silicon as set forth in claim 1, wherein the reactor shell is made of at least one metal selected from carbon steel and stainless steel. 13. The apparatus for preparing granular polysilicon as set forth in claim 1, wherein the reactor tube is made of a single component material or a plurality of materials selected from the group consisting of quartz, silica, silicon nitride, boron nitride, silicon carbide, graphite, glassy carbon, silicon, and a mixture thereof. 14. The apparatus for preparing granular polysilicon as set forth in claim 13, wherein the reactor tube consists of a single layer or a plurality of layers in the thickness direction, each layer of which is made of a different material. 15. The apparatus for preparing granular polysilicon as set forth in claim 1, wherein the internal heater comprises one or a plurality of heater units. 16. The apparatus for preparing granular polysilicon as set forth in claim 15, wherein the plurality of heater units are electrically interconnected in series and/or in parallel. 17. The apparatus for preparing granular polysilicon as set forth in claim 15, wherein the heater unit is electrically connected to a power supply source through an electrical connecting means coupled with the reactor shell. 18. The apparatus for preparing granular polysilicon as set forth in claim 17, wherein the electrical connecting means comprises electrodes installed inside and/or outside of the reactor shell and the heater units are electrically interconnected by the electrode in series and/or in parallel. 19. The apparatus for preparing granular polysilicon as set forth in claim 18, wherein the electrode is made of a metal or an alloy comprising at least one metal element selected from copper (Cu), aluminum (Al) and cadmium (Cd) or is made of graphite, the surface of which is treated as silicon carbide. 20. The apparatus for preparing granular polysilicon as set forth in claim 15, wherein a resistive element which the heater unit comprises and at which electrical resistance heating occurs, is in the form of a rod, a wire, a filament, a bar, a strip or a ribbon having circular, elliptical or polygonal cross-section or of a conduit, a tube, a cylinder or a duct having concentric circular, elliptical or polygonal cross-section, with the shape and/or dimension of the cross-section being uniform or variable along the length direction. 21. The apparatus for preparing granular polysilicon as set forth in claim 20, wherein the resistive element is made of one or two materials selected from graphite, silicon carbide and silicon. 22. The apparatus for preparing granular polysilicon as set forth in claim 20, wherein the resistive element is made of a metal or an alloy selected from the group consisting of tungsten (W), rhenium (Re), osmium (Os), tantalum (Ta), molybdenum (Mo), niobium (Nb), iridium (Ir), ruthenium (Ru), technetium (Tc), hafnium (Hf), rhodium (Rh), vanadium (V), chromium (Cr), zirconium (Zr), platinum (Pt), thorium (Th), lanthanum (La), titanium (Ti), lutetium (Lu), yttrium (Y), iron (Fe), nickel (Ni), magnesium (Mg), aluminum (Al), and a mixture thereof. 23. The apparatus for preparing granular polysilicon as set forth in claim 20, wherein the resistive element is made of a ceramic metal selected from the group consisting of molybdenum silicide (Mo—Si), lanthanum chromite (La—Cr—O), zirconia, and a mixture thereof. 24. The apparatus for preparing granular polysilicon as set forth in claim 20, wherein the heater unit is constructed by installing a protection tube outside the resistive element, forming one or a plurality of separation layers on the surface of the resistive element or installing a protection tube outside the resistive element after forming the separation layer(s) on the resistive element. 25. The apparatus for preparing granular polysilicon as set forth in claim 24, wherein the protection tube has concentric circular, elliptical or polygonal cross-section in the thickness direction. 26. The apparatus for preparing granular polysilicon as set forth in claim 24, wherein at least one of the separation layer and the protection tube comprises 1 to 5 layers, each of which is made of a different barrier component. 27. The apparatus for preparing granular polysilicon as set forth in claim 26, wherein the barrier component comprises a component for preventing impurities from migrating to the silicon particles and/or the fluidizing gas from the resistive element. 28. The apparatus for preparing granular polysilicon as set forth in claim 26, wherein the barrier component comprises an electrically insulating component. 29. The apparatus for preparing granular polysilicon as set forth in claim 26, wherein the barrier component comprises nitride, oxide, carbide or oxynitride of silicon (Si) or boron (B). 30. The apparatus for preparing granular polysilicon as set forth in claim 26, wherein the barrier component comprises nitride, oxide, silicide, boride, carbide, oxynitride or silicon oxide of one or a plurality of metal elements selected from the group consisting of tungsten (W), rhenium (Re), osmium (Os), tantalum (Ta), molybdenum (Mo), niobium (Nb), iridium (Ir), ruthenium (Ru), technetium (Tc), hafnium (Hf), rhodium (Rh), vanadium (V), chromium (Cr), zirconium (Zr), platinum (Pt), thorium (Th), lanthanum (La), titanium (Ti), lutetium (Lu), yttrium (Y), iron (Fe), nickel (Ni), magnesium (Mg), aluminum (Al), and a mixture thereof. 31. The apparatus for preparing granular polysilicon as set forth in claim 26, wherein the thickness of the separation layer is in the range of 1 μm to 5 mm in total and/or the thickness of the protection tube is in the range of 1 mm to 20 mm. 32. The apparatus for preparing granular polysilicon as set forth in claim 26, wherein the separation layer further comprises a silicon layer having a thickness in the range of 1 μm to 5 mm with silicon being the barrier component. 33. The apparatus for preparing granular polysilicon as set forth in claim 1, wherein the reaction gas supplying means exposed to heating zone is constructed in the form of a coaxial multitube in which a reaction gas nozzle for supplying the reaction gas is enclosed by one or a plurality of nozzles. 34. The apparatus for preparing granular polysilicon as set forth in claim 33, wherein an inert gas flows at an annular region of the coaxial multitube. 35. The apparatus for preparing granular polysilicon as set forth in claim 34, wherein hydrogen chloride is added to the inert gas continuously, intermittently or periodically. 36. The apparatus for preparing granular polysilicon as set forth in claim 1, wherein the particle discharging means is constructed in the form of a coaxial multitube along with the reaction gas supplying means or in an independent form separately from the reaction gas supplying means. 37. The apparatus for preparing granular polysilicon as set forth in claim 1, wherein material constituting at least one of the fluidizing gas supplying means, the reaction gas supplying means and the particle discharging means comprises at least one selected from the group consisting of quartz, silica, silicon nitride, boron nitride, silicon carbide, graphite, silicon, glassy carbon, and a mixture thereof. 38. The apparatus for preparing granular polysilicon as set forth in claim 37, wherein at least one of the fluidizing gas supplying means, the reaction gas supplying means and the particle discharging means consists of a single component material, or consists of a plurality of layers in the thickness direction, each layer of which is made of a different material.
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이 특허에 인용된 특허 (13)
Van Slooten Richard A. (E. Aurora NY) Prasad Ravi (E. Amherst NY), Annular heated fluidized bed reactor.
Eichelberger Charles W. (Schenectady NY) Wojnarowski Robert J. (Clifton Park NY), Electrical conductors arranged in multiple layers and preparation thereof.
Kim Hee Y. (Daejeon KRX) Song Yong M. (Daejeon KRX) Jeon Jong Y. (Daejeon KRX) Kwon Dae H. (Daejeon KRX) Lee Kang M. (Daejeon KRX) Lee Jae S. (Daejeon KRX) Park Dong S. (Daejeon KRX), Fluidized bed reactor heated by microwaves.
Kim Hee Y. (Daejeon KRX) Song Yong M. (Daejeon KRX) Jeon Jong Y. (Daejeon KRX) Kwon Dae H. (Daejeon KRX) Lee Kang M. (Daejeon KRX) Lee Jae S. (Daejeon KRX) Park Dong S. (Daejeon KRX), Heating of fluidized bed reactor by microwaves.
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