CN203484138U - Polysilicon fluidized bed reactor - Google Patents
Polysilicon fluidized bed reactor Download PDFInfo
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- CN203484138U CN203484138U CN201320634205.6U CN201320634205U CN203484138U CN 203484138 U CN203484138 U CN 203484138U CN 201320634205 U CN201320634205 U CN 201320634205U CN 203484138 U CN203484138 U CN 203484138U
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Abstract
The utility model relates to a polysilicon fluidized bed reactor which is characterized by comprising a gas exhausting area (1-2), a reaction area (1-1) and a gas buffering area (1-3), wherein the gas exhausting area (1-2) is positioned at the upper part of the reaction area (1-1) and is directly communicated with the reaction area (1-1); the gas buffering area (1-3) is positioned at the lower part of the reaction area (1-1) and is separated from the reaction area (1-1) through a gas distributor (9); a discharging outlet (9-3) through which product particles can be discharged out of the reactor is formed in the center of the gas distributor (9); a hydrogen covering gas inlet (9-1) and a reaction gas inlet (9-2) are formed in the outer circle of the gas distributor (9); a raw material gas inlet (8) and a fluidization gas inlet (10) are formed in the gas buffering area (1-3); a microwave heater (2-4) is arranged on the cylindrical wall of the reaction area (1-1); and a polysilicon seed inlet (3) and a tail gas exhausting outlet (4) are formed in the gas exhausting area (1-2). The polysilicon fluidized bed reactor is simple in structure and cannot generate a wall-adsorption phenomenon.
Description
Technical field
The utility model relates to a kind of semi-conducting material manufacturing equipment, especially a kind of polysilicon manufacturing equipment, specifically a kind of fluidized-bed reactor that utilizes chemical vapour deposition (CVD) principle to prepare granulated polycrystalline silicon.
Background technology
At present, Siemens Method and improved Siemens are the production methods having comparative advantage at present.Siemens Method by being heated to approximately 1100 ℃ with electrode by silicon rod in CVD reactor, and trichlorosilane, at silicon rod Surface disintegration, deposits crystalline silicon.
But there is the problem that energy consumption is high and pollution is heavy in Siemens Method, its reason has: (1) Siemens Method is produced polysilicon, low conversion rate, and energy consumption is high; (2) the method produces a large amount of silicon tetrachloride byproducts, and this byproduct is difficult to recycle, and causes severe environmental pollution.
Improved Siemens has increased the retracting device of by-product silicon tetrachloride, solved the recovery problem of by-product silicon tetrachloride, pollution abatement, but this method need to be carried out in HTHP thermal response still, consume large-tonnage product polysilicon, apparatus expensive, course of reaction danger are high simultaneously.
For overcoming the inherent shortcoming of Siemens Method, developed the substitute technologies such as silane fluidized bed process, metal replacement method and Physical Metallurgy method both at home and abroad, wherein fluidized bed process is own through obtaining commercial Application America and Europe, but China is still in the research primary stage at present.In fluidized bed process, the mixture that passes into unstripped gas and fluidized gas from reactor lower part makes bed fluidisation, elemental silicon is deposited on polycrysalline silcon surface, polysilicon fine grained as crystal seed is connected or is joined off and in fluid bed, the polycrysalline silcon that particle diameter increases is taken out by reactor lower part as product, fluidized-bed reactor is produced the drawback that polysilicon has fundamentally overcome Siemens Method, becomes the focus of research and development in industry.
But fluidized bed reactor equipment has run into problems, sum up as follows: 1. reactor wall deposits.Siliceous deposits reaction does not occur over just on silicon grain, and when the temperature of reactor reaches reaction temperature, the grain silicon of generation can be deposited on reactor wall, causes reactor wall siliceous deposits, affects heat transfer property and product purity.2. in reactor, gas flow rate is controlled.Reacting gas is controlled bad, easily causes reaction not carry out smoothly, easily occurs channel, reacts unequal problem.3. product purity.Because reaction needed is carried out under hot conditions, so the selection of reactor wall material is proposed to very high requirement, needs inner lining material under hot conditions on the one hand, non-volatile impurity effect product purity, need inner lining material can not be out of shape because of variations in temperature on the one hand, avoid frequent replacing.
Summary of the invention
The purpose of this utility model is the attached wall that exists while manufacturing polycrysalline silcon for existing fluidized bed process, reacts unequal problem, designs a kind of polysilicon fluidized-bed reactor that utilizes heating using microwave and hydrogen to cover to improve polysilicon preparation efficiency and quality.
The technical solution of the utility model is:
A kind of polysilicon fluidized-bed reactor, it is characterized in that it is by gas discharge area 1-2, reaction zone 1-1 and gas buffer region 1-3 form, gas discharge area 1-2 is positioned at the top of reaction zone 1-1 and is directly communicated with, gas buffer region 1-3 is positioned at the bottom of reaction zone 1-1, by gas distributor 9, cut apart between the two, the center of gas distributor 9 is provided with product particle and discharges the discharging opening 9-3 outside reactor, discharging opening 9-3 is connected with the outlet 7 stretching out outside reactor, in the outer ring of gas distributor 9, be provided with for hydrogen blanketing gas and enter reaction zone inwall and reduce the hydrogen coating gas import 9-1 that inwall silicon grain deposits, hydrogen coating gas import 9-1 is connected with the hydrogen gas pipe 6 stretching out outside reactor, on the gas distributor 9 between discharging opening 9-3 and hydrogen coating gas import 9-1, be provided with the reaction gas inlet 9-2 being connected with gas buffer region, on the 1-3 of gas buffer region, be provided with raw material gas inlet 8 and fluidizing gas import 10, unstripped gas lower than reaction temperature enters reaction zone 1-1 in speed and the ratio set from raw material air inlet 8 enters buffering area under the control of gas distributor 9, the barrel of reaction zone 1-1 is provided with microwave applicator 2-4, gas discharge area 1-2 is provided with crystal seed entrance 3 and tail gas outlet 4, on tail gas outlet 4, cyclone separator is installed, for separating of tail gas and unreacted silica soot.
Described gas distributor 9 is doctor's cone cap shape structure, is provided with hydrogen coating gas import 9-1, reaction gas inlet 9-2 and discharging opening 9-3.
The reaction gas inlet 9-2 structure of described gas distributor 9 is direct piping shape or horn mouth shape or convergent-divergent shape (Venturi type).Outlet section in tri-kinds of shapes of gas import 9-2 can be opened straight trough road or sawtooth conduit.
Described reactor wall 2 is located in the wall corresponding with reaction zone 1-1, the inwall of reaction zone is provided with coat of silicon carbide 2-5 and microwave applicator 2-4, between the outer wall 2-1 of reaction zone and microwave applicator 2-4, be provided with thermal insulation layer 2-2 and microwave reflection layer 2-3, wherein microwave reflection layer 2-3 and microwave applicator 2-4 next-door neighbour.
The beneficial effects of the utility model:
Reactor of the present utility model is fluidized-bed reactor, and wherein reactor is divided into gas discharge area from top to bottom, reaction zone and gas buffer region.Gas discharge area is equipped with cyclone separator, for separating of tail gas and unreacted silica soot; Reaction zone is positioned at the centre of reactor, for chemical reaction and polycrysalline silcon deposition; Gas buffer region is positioned at reaction zone below, for buffering reaction gas and fluidizing gas; Gas distributor is positioned at gas buffer region and reaction zone middle part, and gas distributor is cone cap shape; Heater is microwave applicator, is positioned at reactor reaction zone wall.
The utility model heater is microwave applicator, and reactor shape is tubular, covers on the wall of reactor reaction zone.Inwall scribbles the inorganic ceramic material of carborundum or other penetrable microwaves, and heater is outwards respectively microwave reflection material, heat preserving and insulating material and metal material.After reacting gas, fluidizing gas and silicon seed preheating, enter reactor, so the major function of heater is concurrent heating, make temperature in reaction zone reach reaction temperature required, reduce energy consumption.
Gas buffer region of the present utility model is positioned at the below of reaction zone, and it act as buffering reaction gas.Reacting gas after preheating proportionally enters buffering area, then enters reaction zone.Advantage is: by controlling the proportion control reaction rate of reacting gas, the convenient control of reacting gas gas speed after buffering, avoids the problem of fluidisation inequality in fluid bed.Save a large amount of reactor feed gas, the reacting gas after preheating does not reach reaction temperature, so buffering area does not exist the problem of siliceous deposits.
Gas distributor of the present utility model comprises the import of hydrogen blanketing gas and reacting gas inlet.The import of hydrogen coating gas is positioned at distributor and reactor wall junction, guarantees that the reacting gas concentration of reactor wall is extremely low, effectively reduces silicon grain and is deposited on reactor wall.Reacting gas inlet is positioned at the zone line of gas distributor, for passing into the reacting gas of preheating.
Gas distributor of the present utility model is oblique to be arranged in reactor, and products export is located at the centre of gas distributor, and the oblique distributor that arranges is conducive to take out product particle silicon, in addition, is conducive to buffering reaction gas, to control reacting gas flow velocity.
Reactor feed gas of the present utility model is silane or trichlorosilane, and fluidizing gas is hydrogen, and two kinds of gases enter buffering area, are mixed into reacting gas.Hydrogen coating gas is hydrogen, enters reaction zone, forms shielding gas flow, makes reactor wall reacting gas concentration extremely low, prevents that siliceous deposits is on wall.
The utility model is simple in structure, rationally distributed, can not produce the problem that now existing fluidized-bed reactor exists, and especially can not produce attached wall phenomenon, and reacting gas is controlled convenient, can guarantee to react to carry out smoothly, there will not be channel, reacts unequal problem.Product purity can improve more than 30%.
Accompanying drawing explanation
Fig. 1 is overall structure schematic diagram of the present utility model.
Fig. 2 is the top view of gas distributor.
Fig. 3 is the sectional view of gas distributor.
Fig. 4 is reactor reaction zone wall sectional view.
Wherein, 1-1: reaction zone; 1-2: gas discharge area; 1-3: gas buffer region; 2: reaction zone wall; 3: crystal seed entrance; 4-tail gas outlet; 5: grain silicon; 6: the import of hydrogen blanketing gas; 7: grain silicon outlet; 8: raw material gas inlet; 9: gas distributor, 10: fluidizing gas import; 9-1: hydrogen coating gas import; 9-2: reacting gas inlet; 9-3: grain silicon outlet; 2-1: reactor reaction zone outer wall, 2-2: thermal insulation layer, 2-3: microwave reflection material, 2-4: microwave applicator, 2-5: coat of silicon carbide.
The specific embodiment
Below in conjunction with drawings and Examples, the utility model is further described.
As Figure 1-4.
A kind of polysilicon fluidized-bed reactor, it is by gas discharge area 1-2, reaction zone 1-1 and gas buffer region 1-3 form, as shown in Figure 1, gas discharge area 1-2 is positioned at the top of reaction zone 1-1 and is directly communicated with, gas buffer region 1-3 is positioned at the bottom of reaction zone 1-1, by the gas distributor 9 of doctor's cone cap shape structure, cut apart between the two, as Fig. 3, shown in 4, gas divides and the center of device 9 is provided with and discharges the discharging opening 9-3 outside reactor for product particle, discharging opening 9-3 is connected with the outlet 7 stretching out outside reactor, in the outer ring of gas distributor 9, be provided with the hydrogen coating gas import 9-1 that hydrogen supply coating gas enters reaction zone inwall and reduces inwall silicon grain deposition, hydrogen coating gas import 9-1 is connected with the hydrogen gas pipe 6 stretching out outside reactor, on the gas distributor 9 between discharging opening 9-3 and hydrogen coating gas import 9-1, be provided with the reaction gas inlet 9-2 being connected with gas buffer region, according to material characteristic reaction gas inlet 9-2 structure, can be direct piping shape, horn mouth shape or convergent-divergent shape (Venturi type).Outlet section in tri-kinds of shapes of gas import 9-2 can be opened straight trough road or sawtooth conduit.On the 1-3 of gas buffer region, be provided with raw material gas inlet 8 and fluidizing gas import 10, unstripped gas lower than reaction temperature enters reaction zone 1-1 in speed and the ratio set from raw material air inlet 8 enters buffering area under the control of gas distributor 9, the barrel of reaction zone 1-1 is provided with microwave applicator 2-4, described microwave applicator 2-4 is arranged in the wall corresponding with reaction zone 1-1, the inwall of reaction zone is provided with coat of silicon carbide 2-5, between the outer wall 2-1 of reaction zone and microwave applicator 2-4, be provided with thermal insulation layer 2-2 and microwave reflection layer 2-3, wherein microwave reflection layer 2-3 and microwave applicator 2-4 are close to, as shown in Figure 4, gas discharge area 1-2 is provided with crystal seed entrance 3 and tail gas outlet 4, on tail gas outlet 4, cyclone separator is installed, for separating of tail gas and unreacted silica soot.
Details are as follows:
Polysilicon fluidized-bed reactor of the present utility model order is from top to bottom respectively: gas discharge area 1-2, reaction zone 1-1 and gas buffer region 1-3.Gas buffer region 1-3,1-1 separates with reaction zone.Upper side at reactor arranges crystal seed entrance 3 and exhaust emissions outlet 4, in novel fluidized bed reactor bottom side, sulfiding gas import 10 and unstrpped gas import 8 are set, unstrpped gas is proportionally sent into after buffering area 1-3 mixing after preheating, enters reaction zone 1-1 reaction and forms grain silicon 5.At Novel fluidization bed bioreactor middle part, reactor wall adopts heating using microwave, and in microwave applicator 2-4 insertion reaction device reaction zone wall 2, reactor wall arranges coat of silicon carbide 2-5.Gas distributor 9 is positioned in the middle of reaction zone and buffering area, and distributor periphery passes into hydrogen 6, forms hydrogen blanket protection wall, and bottom, distributor centre arranges product particle silicon outlet 7.The reacting gas of preheating 8,10 is proportionally added to buffering area, enter reaction zone after mixing, the setting of buffering area is to adjust extent of reaction, controls gas flow rate.Heater of the present utility model is the microwave applicator 2-4 being embedded in reaction zone wall, is mainly used in concurrent heating, is shaped as cylindricly, and wall 2 comprises outer wall 2-1, thermal insulation layer 2-2, microwave reflection material 2-3, microwave applicator 2-4 and coating 2-5, as Fig. 4.Gas distributor 9 is for bullet and open a plurality of distribution holes, and gas distributor is arranged at heated buffer zone and reaction zone middle part.Outer ring is hydrogen shield, and hydrogen shield import can be a plurality of, as Fig. 2.
Concrete example 1: reactor feed gas hydrogen and trichlorosilane are preheated to respectively to 700-800 ℃, are passed in gas buffer region, hydrogen coating gas is passed in reactor simultaneously.Utilize gas distributor 9 that hydrogen partial is passed in reaction zone 1-1 along wall, with feed arrangement, the polysilicon crystal seed that is preheated to 1000-1100 ℃ is passed into reaction zone from import 3, now at the low suspension that blows of reacting gas, by heater, the temperature of polysilicon crystal seed is remained on to 1000-1100 ℃, now, hydrogen starts to reduce trichlorosilane under the atmosphere of 1000-1100 ℃, the polysilicon producing is ceaselessly gathered on polysilicon crystal seed, carrying out along with reaction, polycrysalline silcon constantly increases to after technique initialization size, because Action of Gravity Field drops down onto product collecting device.Product collecting device is filled with inert gas, oxidized with the product of solar heat protection.Waste gas, the unreacted silicon seed that reaction produces or the silicon grain that does not reach requirement enter cyclone separator and carry out separation, and crystal seed and gas are reusable.
Concrete example 2: pass into gas buffer region after reactor silane is preheated to 500-600 ℃, simultaneously hydrogen coating gas is by the gas distributor reaction zone of entering.Utilize gas distributor 8 that hydrogen partial is passed into reaction zone along reactor wall, with feed arrangement, the silicon seed that is preheated to 700-800 ℃ is introduced to reaction zone, now at reacting gas, blow low suspension in reaction zone, by heater, make the surface temperature of seed particles remain on 700-800 ℃, pass into silane gas, now silane gas issues raw decomposition reaction the atmosphere of 700-800 ℃, decomposes and produces silicon and hydrogen.The silicon producing is constantly deposited on the surface of silicon seed, and along with the carrying out of reaction, silicon grain constantly increases to technique initialization size, by Action of Gravity Field, falls into product collecting device, is filled with inert gas again oxidized with the silicon grain of solar heat protection in product collecting device.The hydrogen producing is being carried the unreacted silicon seed of part secretly and is being entered cyclone separator, and the silicon that separation obtains and hydrogen repetitive cycling are used.
The utility model does not relate to partly all prior aries that maybe can adopt same as the prior art to be realized.
Claims (4)
1. a polysilicon fluidized-bed reactor, it is characterized in that it is by gas discharge area (1-2), reaction zone (1-1) and gas buffer region (1-3) form, gas discharge area (1-2) is positioned at the top of reaction zone (1-1) and is directly communicated with, gas buffer region (1-3) is positioned at the bottom of reaction zone (1-1), by gas distributor (9), cut apart between the two, the center of gas distributor (9) is provided with product particle and discharges the discharging opening (9-3) outside reactor, discharging opening (9-3) is connected with the outlet (7) stretching out outside reactor, in the outer ring of gas distributor (9), be provided with for hydrogen blanketing gas and enter reaction zone inwall and reduce the hydrogen coating gas import (9-1) that inwall silicon grain deposits, hydrogen coating gas import (9-1) is connected with the hydrogen gas pipe (6) stretching out outside reactor, on the gas distributor (9) between discharging opening (9-3) and hydrogen coating gas import (9-1), be provided with the reaction gas inlet (9-2) being connected with gas buffer region, on gas buffer region (1-3), be provided with raw material gas inlet (8) and fluidizing gas import (10), unstripped gas lower than reaction temperature enters reaction zone (1-1) in speed and the ratio set from raw material air inlet (8) enters buffering area under the control of gas distributor (9), the barrel of reaction zone (1-1) is provided with microwave applicator (2-4), gas discharge area (1-2) is provided with crystal seed entrance (3) and tail gas outlet (4), tail gas outlet is provided with cyclone separator on (4), for separating of tail gas and unreacted silica soot.
2. reactor according to claim 1, is characterized in that described gas distributor (9) is doctor's cone cap shape structure, is provided with hydrogen coating gas import (9-1), reaction gas inlet (9-2) and discharging opening (9-3).
3. reactor according to claim 1, is characterized in that reaction gas inlet (9-2) structure of described gas distributor (9) is direct piping shape or horn mouth shape or convergent-divergent shape; Outlet section in three kinds of shapes of gas import (9-2) has straight trough road or sawtooth conduit.
4. reactor according to claim 1, it is characterized in that described reactor wall (2) is located in the wall corresponding with reaction zone (1-1), the inwall of reaction zone is provided with coat of silicon carbide (2-5) and microwave applicator (2-4), between the outer wall (2-1) of reaction zone and microwave applicator (2-4), be provided with thermal insulation layer (2-2) and microwave reflection layer (2-3), wherein microwave reflection layer (2-3) and microwave applicator (2-4) next-door neighbour.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201320634205.6U CN203484138U (en) | 2013-10-15 | 2013-10-15 | Polysilicon fluidized bed reactor |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201320634205.6U CN203484138U (en) | 2013-10-15 | 2013-10-15 | Polysilicon fluidized bed reactor |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103495366A (en) * | 2013-10-15 | 2014-01-08 | 江苏中圣高科技产业有限公司 | Granular polycrystalline silicon fluidized bed reactor |
| CN108778493A (en) * | 2016-02-27 | 2018-11-09 | 学校法人早稻田大学 | The manufacturing method of particle processing unit and catalyst loading body and/or fibrous carbon nanostructure |
| CN117105230A (en) * | 2023-08-25 | 2023-11-24 | 乐山协鑫新能源科技有限公司 | Method and device for producing granular polycrystalline silicon |
-
2013
- 2013-10-15 CN CN201320634205.6U patent/CN203484138U/en not_active Withdrawn - After Issue
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103495366A (en) * | 2013-10-15 | 2014-01-08 | 江苏中圣高科技产业有限公司 | Granular polycrystalline silicon fluidized bed reactor |
| CN108778493A (en) * | 2016-02-27 | 2018-11-09 | 学校法人早稻田大学 | The manufacturing method of particle processing unit and catalyst loading body and/or fibrous carbon nanostructure |
| CN108778493B (en) * | 2016-02-27 | 2022-02-11 | 学校法人早稻田大学 | Particle processing device and method for producing catalyst support and/or fibrous carbon nanostructure |
| CN117105230A (en) * | 2023-08-25 | 2023-11-24 | 乐山协鑫新能源科技有限公司 | Method and device for producing granular polycrystalline silicon |
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