CN206108909U - Liquid silicon apparatus for producing - Google Patents

Abstract

The utility model discloses a liquid silicon apparatus for producing, the device exists gaseous condensing zone, liquid drop formation region and liquid drop growth region including the plasma generator, reactor, silicon liquid loader and the tail gas piece -rate system that connect gradually at reactor in proper order. Adopt the utility model discloses an apparatus for producing can directly obtain high -purity liquid silicon materials, and operation is simple, and permits liquid silicon materials directly to carry the ingot casting process in low reaches, vertical pulling single crystal process and perhaps prepare processes such as silicon chip, can greatly reduce polycrystalline silicon production investment cost, guarantees the stable long period run of apparatus for producing, increase of production.

Description

Liquid silicon manufacturing apparatus

Technical field

This utility model is related to a kind of preparation facilitiess of polycrystalline silicon material, and in particular to a kind of liquid silicon manufacturing apparatus.

Background technology

Existing method for preparing polysilicon mainly includes improvement Siemens process or fluidized-bed process, wherein improveing Siemens The polysilicon of technique productions accounts for more than 85%, technological principle with chlorosilane and hydrogen as raw material, in reduction furnace reactor Silicon wicking surface, the reaction production polysilicon at a temperature of 1000-1200 DEG C.Polycrystalline silicon reducing furnace needs high pressure resistant, high temperature and corrosion Property gas, furnace tube and chassis need to design cooling water flow conduits, and flow out enough positions for air inlet, offgas outlet and electrode, if Standby manufacture difficulty is big.After equipment enlarging, although can improve single stove production capacity, but the manufacture difficulty of equipment is also increased, and is virtually increased Product cost is added.In addition, the equipment is intermittent production, after the completion of heat growth, blowing out is needed, cooled down, torn rod, blowing out open Time is approximately 1/5th of production time, causes single stove annual capacity limited.

The principle of fluidized-bed process be with silane and hydrogen as raw material, in a fluidized bed reactor, 400-600 DEG C of temperature Under, in seed crystal face formation of deposits grain silicon, when grain silicon is grown up to certain particle diameter, discharge from products export and obtain product. The operation difficulty of fluid bed main equipment is the fluidized state of the stable bed of control, it is to avoid local hooks stream with bubbling phenomenon Occur, further, since fluid bed mode of heating is more based on radiation or sensing heating, therefore, will in bed body internal cross section Thermograde is formed, especially for the fluid bed of major diameter, thermograde phenomenon becomes apparent from.

The Chinese patent of Patent No. ZL200780033206.2 discloses a kind of plasma for manufacturing polysilicon Precipitation equipment and method, the device includes the room of deposit polycrystalline silicon and the exhaust system for reclaiming non-deposition gases, inductance coupling Close plasma torch and produce and be basically perpendicular to the plasma flame of deposition surface, so as to deposit polycrystalline silicon across the deposition surface Layer.The Chinese patent of Patent No. 200910204974.0 discloses a kind of method that utilization hydrogen plasma produces polysilicon, The method adopts one or more in dichlorosilane, silicochloroform and Silicon chloride. for unstrpped gas, and adopts hydrogen As reducing gas, or add one or more in helium, neon, argon and Krypton in addition as auxiliary gas, with raw material Simultaneously plasma is converted to by plasma producing apparatus after gas mixing, in being then delivered to reduction furnace, in reduction furnace Polysilicon is deposited on interior silicon core.

Number of patent application is that 201010246191.1 Chinese patent discloses a kind of tetrafluoride reduced by plasmas life The method for producing polysilicon, including being passed through the plasma reactor that has been filled with hydrogen after raw material silicon tetrafluoride gas and hydrogen mixing It is interior, in the presence of plasma, silicon tetrafluoride gas and hydrogen moment be heated to 1200 DEG C～3500 DEG C it is concurrent biochemical Reaction, generates polysilicon solid and hydrogen fluoride gas.It is many that the Chinese patent of Patent No. 201010559873.8 discloses one kind Crystal silicon process units and method, device includes that polysilicon solidification receives container, microwave surface wave plasma torch, polysilicon solidification Receive the polysilicon that container reception microwave surface wave plasma torch is generated.Method is using SiHCl3 steam and the gas conducts of H 2 Raw material reaction thing, the raw material reaction in being discharged raw material reaction thing to heat medium tube by microwave surface wave plasma torch Thing, the silicon of generation cools down in polysilicon solidification receives container and solidifies and obtain polysilicon.

Existing polysilicon prepares patent and although mentions plasma heating technology, but plasma generator is only limited the use of In heating unstripped gas so as to decompose and produce polysilicon and be deposited on carrier, product, plasma technique institute are collected in final cooling The huge heat for producing loses in vain, causes energy dissipation.

Number of patent application is that 200710063653.4 Chinese patent discloses a kind of plasma producing method of polysilicon And its device, described device contains plasma switch room, and unstripped gas heater produces flame passes using high-frequency electric field Earthenware duct, the electric heating thermal insulation crucible of collection liquid monomer silicon, conversion chamber wall temperature detecting system, temperature lowering water anchor ring system, with And tail gas separation tower.Though the patent refers to the preparation and collection of liquid-state silicon, by simple plasma flame and earthenware duct It is difficult to raw material is fully converted to into liquid-state silicon as described in patent collect, and major part will be in superfine silica powder form from tail Discharge in gas system, this considerably increases material loss.

Therefore, a kind of new liquid silicon manufacturing apparatus are still required for, drawbacks described above is overcome, can be to most of silicon matter Liquid collection is carried out, and suppresses silicon matter to form silicon powder to discharge from exhaust system；Equipment can be met again simple, operating procedure letter It is single, can quantity-produced requirement.

The content of the invention

Goal of the invention：Primary technical problem to be solved by this invention is to overcome production of polysilicon equipment system in prior art The deficiency that complex process, input are high, controlling of production process is difficult, operation difficulty is big is made, the present invention provides a kind of new preparation The generating means of liquid-state silicon, using this technical scheme, can directly obtain high purity liquid state silicon materials, and operation sequence is simple, and permits Perhaps liquid silicon material is delivered directly to the ingot casting operation in downstream, pulling of crystals operation or prepares the operations such as silicon chip, can be very big Reduce production of polysilicon cost of investment, it is ensured that the stable long-term operation of process units, improve yield.

To solve above-mentioned primary technical problem, the present invention is adopted the following technical scheme that：

A kind of liquid silicon manufacturing apparatus, including plasma generator, reactor, silicon liquid carrier and tail gas separation equipment, The outlet of the plasma generator connects with the import of the reactor, the outlet of the reactor and the silicon liquid carrier Entrance connect, the offgas outlet of the silicon liquid carrier connects with the tail gas separation system.

Preferably, the plasma generator is using known radio frequency induction plasma source, direct plasma source, micro- Ripple plasma source etc., it is further preferred that the plasma generator adopts rf induction plasma source, in plasma Heart temperature 2000-10000 DEG C.

Preferably, the plasma generator has laterally attached unstripped gas air inlet, carrier gas air inlet and waits Gas ions work gas air inlet, is connected by each independent air inlet pipe with generator.

Preferably, the reactor has the diameter bigger than the plasma generator, and with big draw ratio, institute The draw ratio for stating reactor is more than 3.It is further preferred that the reactor top is cylinder straight-tube shape, bottom is coniform.

Preferably, there is gas condensing zone, droplet formation area and droplet growth area successively in the reactor, further Preferably, the gas condensing zone is present in the Reactor inlet peripheral region, and the droplet formation area is present in reactor Upper area, the droplet growth area is present in reactor lower part region, and above three region has no strict differentiation, can be according to The actual flow locations of atomic state material are determining its distribution in reactor, it is contemplated that the factor of air-flow entrainment, same In region, while allowing the material that there is different shape.

Preferably, the import of the reactor is located at reactor head side, there is tangential rotating channel to set for the import Meter.It is further preferred that the tangential entry quantity of the reactor is 1-6, when import volume is even number, all imports are equal It is presented symmetrical along reactor axial direction, and along the longitudinally asymmetric distribution of reactor.

Preferably, the reactor outer wall is provided with many pipelines, the pipeline can be set along reactor is axially vertical Put in reactor outer wall, can be around reactor cross-section disk in reactor outer wall.Cooling medium can be passed through in the pipeline Or adding thermal medium, cooling medium can be using cooling water pressure, low-pressure steam or conduction oil be added, and the temperature of cooling medium is normal Temperature, plus thermal medium can be using low-pressure steam or conduction oil.Being actually needed according to reactor, when cooling is needed, can be to pipe Cooling medium is conveyed in road, when heating is needed, can be conveyed into pipeline plus thermal medium.

It is further preferred that the bottom of the reactor is in infundibulate, and heater is provided with, heating-up temperature is maintained at More than 1500 degree.It is further preferred that the heater is induction heating apparatus, electric heater unit or resistive heating device.

Preferably, there is the reactor laterally attached unstripped gas air inlet, carrier gas air inlet and plasma (orifice) gas to enter QI KOU, is connected by each independent air inlet pipe with reactor.

Preferably, the reactor wall is coated with least one in quartz, silicon nitride, carborundum or silicon coating.

Preferably, the tail gas separation equipment is selected from cyclone separator or bag-type dust removal system.It is further preferred that institute Stating tail gas separation equipment has two, is followed successively by cyclone separator and bag-type dust removal system.Still more preferably, the silicon liquid is held Carry and filter is additionally provided between device and the tail gas separation equipment, the filter is bag filter.

Preferably, the silicon liquid carrier is made up of crucible, firing equipment and lagging casing.

It is further preferred that the silicon liquid carrier also has pod apertures, pod apertures are set by mozzle with pulling of crystals Standby or casting unit prepares silicon chip equipment and is connected.

Wherein, the exotic material such as the material selection graphite of the reactor, metal alloy, ceramics or other alloying metals In at least one, but not limited to this.

Wherein, the reactor also includes heat-insulation layer, and the heat-insulation layer is by ceramics or at least one in C-C composite Heat-barrier material is constituted.

Beneficial effect：

Liquid silicon manufacturing apparatus of the invention, due to having carried out split plot design to reactor, make to be performed containing silicon materials The production procedure of the silicon liquid drop-silicon liquid of atomic state material-small silicon liquid drop-larger, and liquid receipts are carried out to most of silicon matter Collection, can directly obtain high purity liquid state silicon materials, and operation sequence is simple, it is to avoid produce chunk polysilicon or granulated polycrystalline silicon The operation that product are crushed and melted, shortens technological process and operation, improves product purity.

Liquid silicon manufacturing apparatus of the invention, it is allowed to which liquid silicon material product is delivered directly to into the pourer in downstream Sequence, pulling of crystals operation prepare the operations such as silicon chip, can greatly reduce production of polysilicon cost of investment, and ensure that The stable long-term operation of process units, without the need for stopping product is taken out, and improves the yearly productive capacity of production efficiency and process units.

Liquid silicon manufacturing apparatus of the invention, reactor enters material anti-using the design of angential admission mode After answering area, can be fully contacted with reactor wall, increase gas phase disturbance extends condensing zone, drop shape of the material in reactor Into area and the time of staying in droplet growth area, promote the fast-growth of silicon liquid drop；

Liquid silicon manufacturing apparatus of the invention, by cyclone separator and the use in conjunction of bag-type dust removal system, will Tail gas in tail gas is respectively processed recovery with silicon powder, and is introduced in silicon liquid carrier and plasma generator, realizes Recycling for by-product material, reduces environmental pollution；

Liquid silicon manufacturing apparatus of the invention are follow-up continuous crystal-pulling, melting ingot casting and direct silicon chip technology Exploitation provides sufficient liquid silicon materials supply, such as the liquid-state silicon prepared by the present invention can combine with czochralski crystal growing furnace and be connected Continuous crystal-pulling, improves crystal-pulling efficiency, also can combine with ingot furnace, reduces broken and reheating melting the energy of silicon cooling and damages Consumption, also can be combined, by liquid-state silicon direct growth silicon chip with direct epitaxy technology.

Except invention described above solve technical problem, constitute technical scheme technical characteristic and by these skills Outside the advantage that the technical characteristic of art scheme is brought, the present invention liquid silicon manufacturing apparatus can solve other technologies problem, The advantage that the other technical characteristics included in technical scheme and these technical characteristics bring, will combine accompanying drawing and make further in detail Thin explanation.

Description of the drawings

Fig. 1 is the schematic diagram of liquid silicon manufacturing apparatus of the present invention；

Fig. 2 is the Section A-A figure of Fig. 1；

In figure：1 plasma generator, 2 reactors, 201 material resolvers, 202 gas condensing zones, 203 droplet formations Area, 204 droplet growth areas, 3 silicon liquid carriers, 4 tail gas separation systems.

Specific embodiment

The specific embodiment of the present invention is described in detail below in conjunction with the accompanying drawings, but, it is necessary to explanation, this Bright protection domain is not limited to these specific embodiments, involved concrete structure, connection in specific embodiment Mode and technological parameter are to enumerate in this embodiment to illustrate the invention, are not any limit to the present invention System.The scope that the present invention is protected, is determined by claims.

As depicted in figs. 1 and 2, liquid silicon manufacturing apparatus, including plasma generator 1, reactor 2, the and of silicon liquid carrier 3 Tail gas separation equipment 4, the outlet of the plasma generator 1 connects with the import of the reactor 2, and the reactor 2 goes out Mouthful connect with the entrance of the silicon liquid carrier 3, the offgas outlet of the silicon liquid carrier 3 and the phase of tail gas separation system 4 Connect.Generally, plasma generator 1 is tightly connected by the form such as securing member or flange connection with reactor 2, and reactor 2 has There is the diameter bigger than plasma generator 1, and with big draw ratio.High-temperature area in plasma generator is material point Solution area 201, the top of reactor 1 is cylinder straight-tube shape, and bottom is coniform.In reactor 1 exist successively gas condensing zone 202, Droplet formation area 203 and droplet growth area 204.

When using, after plasma generator work, the such as argon of the working gas in plasma generator is converted into etc. from Daughter, material decomposes generation silicon ion by plasma bombardment, due to the already out material resolver of product, under temperature is rapid There is condensation, polymerization in drop, atomic state material, and then form small silicon liquid drop, and into droplet growth region, small silicon liquid drops in gas Body condensing zone and droplet formation area are unsuitable long, to avoid droplets from being grown up in horizontal segment deposition, block pipeline.In droplet growth Area, drives drop and reactor wall to form tangential motion by air-flow, increases the collision probability of silicon liquid drop, thus the speed of growth Accelerate, the peripheral helical downdraught in droplet growth area extends the time of staying of the fluid in droplet growth area, makes liquid There is enough time to grow up, in finally entering silicon liquid carrier.Additionally, the size in droplet growth area should ensure that long enough, to increase Small silicon liquid drops in the time of staying in the region, to make silicon liquid drop grow up as far as possible.

It is further preferred that gas condensing zone is present in Reactor inlet peripheral region, droplet formation area is present in reaction Device upper area, droplet growth area is present in reactor lower part region.Still more preferably, above three region has no strictly Distinguish, its distribution in reactor can be determined according to the actual flow locations of atomic state material, it is contemplated that air-flow is carried secretly Factor, in the same area, while allowing the material that there is different shape.For a person skilled in the art, can be with Adjust the intake velocity containing silicon materials and carrier gas to control the time of staying of material in reactor in each region of reactor.

Meanwhile, the import of reactor is located at reactor head side, and there is tangential rotating channel to design for the import.Further Preferably, it is further preferred that the tangential entry quantity of the reactor is 1-6, when import volume is even number, Suo Youjin Mouth is presented symmetrical along reactor axial direction.However, for a person skilled in the art, the quantity of tangential entry Be not limited to this, in addition it is also necessary to according to actual needs, such as the quantity of plasma generator determining, for being big straight when reactor Footpath size, and with multiple plasma generators it is connected when, then the tangential entry of reactor then for multiple, such as is 8 It is individual, 10,12,14 or more.Outside reactor also have cooling jacket, using plus cooling water pressure, low-pressure steam or Used as cooling medium, the temperature of cooling medium is room temperature, certainly, the cooling medium not limited to this of reactor to conduction oil.Reactor With laterally attached unstripped gas air inlet, carrier gas air inlet and plasma (orifice) gas air inlet, by each independent air inlet pipe with Reactor is connected, and this is well-known to those skilled in the art.

Reactor wall is coated with least one in quartz, silicon nitride, carborundum or silicon coating.Reactor outer wall is arranged There are many pipelines, pipeline can exist along reactor axis to reactor outer wall is vertically set on around reactor cross-section disk Reactor outer wall.Cooling medium can be passed through in pipeline or adds thermal medium, cooling medium can be adopted plus cooling water pressure, low pressure Steam or conduction oil, the temperature of cooling medium is room temperature, plus thermal medium can be using low-pressure steam or conduction oil.According to reactor Be actually needed, when cooling is needed, cooling medium can be conveyed into pipeline, when need heating when, can convey into pipeline add Thermal medium.

In a preferred embodiment, the bottom of reactor is in infundibulate, and is provided with heater, and heating-up temperature is maintained at More than 1500 degree.It is further preferred that heater is induction heating apparatus, electric heater unit or resistive heating device.

The droplet growth area of reactor is in infundibulate, and is provided with heater, and heating-up temperature is maintained at more than 1500 degree, with Enough heats are provided.It is further preferred that heater is induction heating apparatus, electric heater unit or resistive heating device. Tail gas separation equipment is selected from cyclone separator or bag-type dust removal system.It is further preferred that tail gas separation equipment has two, successively For cyclone separator and bag-type dust removal system.In practical operation, it was additionally provided between silicon liquid carrier and tail gas separation equipment Filter, filter is bag filter.Silicon liquid carrier is made up of crucible, firing equipment and lagging casing, is received by crucible The silicon liquid of collection drippage, crucible maintains crucible temperature more than more than 1440 DEG C using sensing or resistive heater heats, so that silicon is protected Hold in liquid.In preferred embodiments, tail gas is entered in cyclone separator by the tail gas mouth of silicon liquid carrier, solid In the crucible that grain is entered in silicon liquid carrier Jing after cyclonic separation from bottom, the tail gas after separation enters cloth envelop collector, enters one Step isolates small silica flour, and the silica flour can be imported in the crucible in silicon liquid carrier, also can be packed as other purposes.

It is further preferred that silicon liquid carrier also has pod apertures, following process process is carried out to derive silicon liquid, such as Pod apertures are by mozzle and pulling of crystals equipment or casting unit or prepare silicon chip equipment and be connected, and can combine with czochralski crystal growing furnace Continuous crystal-pulling is carried out, crystal-pulling efficiency is improved, also can be combined with ingot furnace, reduce broken and reheating melting the energy of silicon cooling Amount loss, also can be combined, by liquid-state silicon direct growth silicon chip with direct epitaxy technology.

Additionally, in the exotic material such as the material selection graphite of reactor, metal alloy, ceramics or other alloying metals At least one, but not limited to this.Reactor also includes heat-insulation layer, by ceramics or at least one heat-insulated material in C-C composite Material composition, but not limited to this, such as quartz etc. can play the material of thermal insulation function and should also be as within protection domain, and this is The technological means that those skilled in the art commonly use.

For a person skilled in the art, plasma generator, reactor, silicon liquid carrier and exhaust treatment system Connected mode belong to known technology, be to realize the object of the invention, on process units of the present invention, be additionally provided with corresponding temperature control dress Put, pressure apparatus and flange, valve, instrument etc., this is also that those skilled in the art can adjust or change according to actual condition 's.Therefore embodiments of the present invention are described in detail above in association with accompanying drawing, but the present invention is not limited to described enforcement Mode.For one of ordinary skill in the art, in the range of the principle and technological thought of the present invention, to these embodiment party Formula carries out various changes, modification, replacement and deformation and still falls within protection scope of the present invention.

Claims (10)

1. a kind of liquid silicon manufacturing apparatus, it is characterised in that including plasma generator, reactor, silicon liquid carrier and tail gas Separation equipment, the outlet of the plasma generator connects with the import of the reactor, the outlet of the reactor with it is described The entrance of silicon liquid carrier connects, and the offgas outlet of the silicon liquid carrier connects with the tail gas separation system.

2. liquid silicon manufacturing apparatus according to claim 1, it is characterised in that：The reactor has than the plasma The big diameter of generator, the reactor has big draw ratio.

3. liquid silicon manufacturing apparatus according to claim 1 and 2, it is characterised in that：There is gas successively in the reactor Body condensing zone, droplet formation area and droplet growth area.

4. liquid silicon manufacturing apparatus according to claim 3, it is characterised in that：The import of the reactor is located at reactor There is tangential rotating channel to design for top side, the import.

5. liquid silicon manufacturing apparatus according to claim 4, it is characterised in that：The tangential entry quantity of the reactor is 1-6.

6. liquid silicon manufacturing apparatus according to claim 5, it is characterised in that：The reactor lower part is in infundibulate, and It is provided with heater.

7. liquid silicon manufacturing apparatus according to claim 5, it is characterised in that：The tail gas separation equipment is selected from whirlwind point From device or bag-type dust removal system.

8. liquid silicon manufacturing apparatus according to claim 7, it is characterised in that the tail gas separation equipment has two, according to It is secondary for cyclone separator and bag-type dust removal system.

9. liquid silicon manufacturing apparatus according to claim 5, it is characterised in that：The silicon liquid carrier is by crucible, heating Equipment and lagging casing are constituted.

10. liquid silicon manufacturing apparatus according to claim 9, it is characterised in that：The silicon liquid carrier also has water conservancy diversion Hole, pod apertures are by mozzle and pulling of crystals equipment or casting unit or prepare silicon chip equipment and be connected.