CN103539125B - Medium melting is connected the method for purifying polycrystalline silicon with preliminary directional freeze - Google Patents
Medium melting is connected the method for purifying polycrystalline silicon with preliminary directional freeze Download PDFInfo
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Abstract
The invention belongs to field of polycrystalline silicon purification, be specifically related to a kind of medium melting is connected purifying polycrystalline silicon device and method with preliminary directional freeze.Plumbago crucible sidewall in device body of heater is provided with furnace lining and ruhmkorff coil outward successively, water-cooled ingot pulling mechanism is installed bottom plumbago crucible, and plumbago crucible and water-cooled ingot pulling mechanism are all in furnace lining holds, plumbago crucible top is provided with the cover graphite annulus identical with external diameter size with plumbago crucible internal diameter.Method comprises silicon material and slag agent to react carries out medium melting, remove the boron impurity in silicon material, after medium melting terminates, the cold ingot pulling mechanism of bottom water is adopted to draw the mode of ingot, preliminary directional freeze is carried out to silicon liquid, gathered by metallic impurity in silicon liquid after top removed, control temperature is poured out after silicon ingot is melted completely.Full liquid state is connected medium melting and preliminary directional freeze, saves power consumption 1000 ~ 2000 KWhs/ton; Production cost reduces by 4000 ~ 8000 yuan/ton.In ingot casting, boron impurity content is less than 0.3ppmw; Metallic impurity total content is less than 100ppmw.
Description
Technical field
The invention belongs to field of polycrystalline silicon purification, be specifically related to a kind of medium melting is connected purifying polycrystalline silicon device and method with preliminary directional freeze.
Background technology
World today's energy dilemma and environmental pollution pressure are also deposited, and people are badly in need of cleaning, safety, continuable new forms of energy.Sun power, as meeting the energy required like this, always is the target that people pursue.People are the utilizations of its heat effect to the use of sun power the earliest, but are difficult to the needs meeting modern society completely.Until the discovery of photoresistance, the manufacture of solar cell, the Land use systems that people find sun power new.Silicon is as the most desirable feedstock of solar cell, impurity wherein mainly contains the nonmetallic impuritys such as metallic impurity and B, P such as Fe, Al, Ca, and these impurity elements can reduce the Compound Degree of silicon crystal grain interface photo-generated carrier, and the Compound Degree of photo-generated carrier determines the photoelectric transformation efficiency of solar cell, removing these impurity so effective has vital effect in the application aspect of solar cell.
The development of solar photovoltaic industry depends on the purification to silicon raw material, comprises medium melting, directional freeze, electron beam purification and casting ingot process in the process of metallurgy method purifying polycrystalline silicon.Metallurgy method has development potentiality because possessing simple, the lower-cost advantage of technique.Require that equipment is the simplest with medium melting in all multi-steps, the easiest industrialization promotion.Thus the researching value of medium melting most reality and application prospect.
In traditional medium fusion process, medium melting and directional freeze are the technique that twice are different, remove boron and other metallic impurity respectively.Apparatus for directional solidification is vacuum apparatus, and the production cycle is generally 40 ~ 60h, and the time is longer, and the silicon ingot after directional freeze needs the impurity enriched district of excising top about 20%.In conventional production, understand through supersolidification---fusing---process of resolidification between twice technique, need during this to consume amount of heat, cost is obviously higher.
Summary of the invention
According to above the deficiencies in the prior art, the present invention proposes a kind of medium melting is connected purifying polycrystalline silicon device and method with preliminary directional freeze, in separate unit medium-frequency induction furnace, realize medium melting be connected with the full liquid state of preliminary directional solidification processes, while removal boron impurity, most of metallic impurity can be removed, silicon material is made to reach 4N level, greatly alleviate the purification pressure of subsequent technique, without the need to all completing directional freeze process to entirety, impurity enriched part is poured out by silicon in the liquid state, the tailing saved after solidifying removes process, realize the direct acquisition of 4N low borosilicate material.
A kind of medium melting of the present invention is connected the device of purifying polycrystalline silicon with preliminary directional freeze, plumbago crucible sidewall in body of heater is provided with furnace lining and ruhmkorff coil outward successively, water-cooled water-cooled ingot pulling mechanism is installed bottom plumbago crucible, and plumbago crucible and water-cooled ingot pulling mechanism are all in furnace lining holds, plumbago crucible top is provided with the cover graphite annulus identical with external diameter size with plumbago crucible internal diameter.
The height of cover graphite annulus is preferably 200 ~ 500mm.
A kind of medium melting is connected the method for the device of purifying polycrystalline silicon with preliminary directional freeze, comprise silicon material and slag agent to react and carry out medium melting, remove the boron impurity in silicon material, after medium melting terminates, the cold ingot pulling mechanism of bottom water is adopted to draw the mode of ingot, carry out preliminary directional freeze to silicon liquid, gathered by the metallic impurity in silicon liquid after top removed, control temperature is poured out after silicon ingot is melted completely.
Preferably include following steps:
(1) in plumbago crucible, add 10 ~ 20% and whole silicon material of slag agent quality, after control heating power to silicon material all melts, average mark adds the agent of residue slag for 2 ~ 5 times, control ruhmkorff coil, make smelting temperature be 1600 ~ 1800 DEG C, after melting, upper strata slag agent is all poured in heat resisting iron mould;
(2) repeat above-mentioned medium fusion process 1 ~ 3 time, the new slag agent at every turn added divides 2 ~ 5 times and adds;
(3), after melting terminates, pour in heat resisting iron mould by 80 ~ 90% of last slag agent quality;
(4) regulate ruhmkorff coil, make smelting temperature be, after 1450 ~ 1550 DEG C, carry out preliminary directional freeze, the water-cooled ingot pulling mechanism controlled bottom plumbago crucible pulls down ingot, and top adds cover graphite annulus simultaneously; Stop drawing ingot when silicon liquid accounts for 10 ~ 20% of silicon material, the cold ingot pulling mechanism of quick hypogene water, makes plumbago crucible set back, and after taking off cover graphite annulus, is all poured in cast iron die by supernatant liquid;
(5) control power to pour out after silicon ingot melts completely.
Preferred version is as follows:
Slag agent in step (1) is the mixture of the calcium oxide of arbitrary proportion, Calcium Fluoride (Fluorspan), titanium dioxide, silicon-dioxide and water glass.
Slag agent in step (1) and step (2) and the ratio of silicon material are 1/3 ~ 2/1.
Step (1) and (5) middle heating power are 200 ~ 300kW.
In step (1) and step (2) add slag at every turn after need melting 20 ~ 30min.
In step (4), plant capacity is 150 ~ 250kW.
In step (4), what water-cooled ingot pulling mechanism was downward draws ingot speed to be 4 ~ 6cm/h, and the speed of the cold ingot pulling mechanism of quick hypogene water is 10 ~ 20cm/min.
Preliminary directional freeze of the present invention is different from the directional freeze in normal process, and one is do not need to carry out under vacuum, not high to equipment requirements degree; Two is less demanding to removal of impurities, only needs to do preliminary removal to metallic impurity, still retains a part of metallic impurity in remaining silicon ingot.
In this device, furnace lining is made up of refractory mortar, and its plasticity-is good, and refractoriness is high, bonding strength is high, and stable chemical nature.The furnace lining lengthened makes water-cooled ingot pulling mechanism drive plumbago crucible to move up and down in furnace lining inside, and after drawing ingot, plumbago crucible moves down, and adds cover graphite annulus, and after preventing plumbago crucible from moving down, the refractory masses exposed is heated and excessively empty burning, reduces equipment loss.Medium melting first time add that slag first adds slag agent quality 10 ~ 20%, and then add silicon material, effect is to protect plumbago crucible.Stop drawing ingot when silicon liquid accounts for 10 ~ 20% of silicon material, the cold ingot pulling mechanism of quick hypogene water, plumbago crucible is set back, after taking off cover graphite annulus, supernatant liquid is poured in cast iron die, this upper strata 10 ~ 20% silicon liquid in impurity enriched degree higher, treatment process is before after all being solidified by silicon material, the silicon material of impurity is rich on excision upper strata, but adopt apparatus of the present invention and method, decrease the step of all solidifying rear excision, directly supernatant liquid is poured out, decrease current consumption, production cost also reduces greatly.Meanwhile, the slag agent of pouring out in operation is collected in cast iron die, can for melting again.
The invention has the advantages that: complete liquid linking medium melting and preliminary directional solidification processes, save power consumption 1000 ~ 2000 KWhs/ton; Medium melting production cost reduces by 4000 ~ 8000 yuan/ton.In ingot casting, boron impurity content is less than 0.3ppmw; After purifying, ingot casting purity is at more than 4N.Metallic impurity total content is less than 100ppmw.
Accompanying drawing explanation
Fig. 1 is that medium melting is connected purifying polycrystalline silicon device with preliminary directional freeze uses schematic diagram.
In figure 1, cover graphite annulus, 2, plumbago crucible, 3, upper strata slag agent, 4, silicon material, 5, ruhmkorff coil, 6, water-cooled ingot pulling mechanism, 7 furnace linings.
Embodiment
Describe the present invention in detail below in conjunction with embodiment, but the present invention is not limited to specific embodiment.
Embodiment 1:
Install furnace lining 7 and ruhmkorff coil 5 from inside to outside successively in body of heater, plumbago crucible 2 is put in furnace lining 7, water-cooled ingot pulling mechanism 6 is installed bottom plumbago crucible 2, and plumbago crucible 2 and water-cooled ingot pulling mechanism 6 are all in the holding of furnace lining 7.
In plumbago crucible 2, add slag agent total mass is 50kg, first 2kg titanium dioxide is added, 2kg silicon-dioxide, the water glass of 2kg Calcium Fluoride (Fluorspan) and 4kg, add 100kg silicon material 4, regulate ruhmkorff coil 5, make heating power be after 200kW to silicon material 4 all fusing, divide and add the agent of residue 40kg slag for 2 times, add melting 20min after slag at every turn, regulate ruhmkorff coil 5, make smelting temperature be 1800 DEG C, then upper strata slag agent 3 is all poured in heat resisting iron mould.
Get and composition in above-mentioned steps and new slag agent 50kg identical in quality, average mark adds in plumbago crucible 2 times, and smelting temperature is 1600 DEG C, upper strata slag agent is all poured in heat resisting iron mould after melting.
Get the new slag agent of 50kg 1 part, repeat second step once; After melting terminates, 40kg upper strata slag agent 3 is poured in heat resisting iron mould.
Adjustment plant capacity is 150kW, and controlling smelting temperature is, after 1450 DEG C, carry out preliminary directional freeze.The water-cooled ingot pulling mechanism 6 controlled bottom plumbago crucible 2 pulls down ingot, draws ingot speed to be 4cm/h, and top adds cover graphite annulus 1 simultaneously, and the height of cover graphite annulus 1 is 200mm.Stop drawing ingot when silicon liquid accounts for 10% of silicon material, water-cooled ingot pulling mechanism 6 fast lift velocity is 10cm/min, plumbago crucible 2 is set back, after taking off cover graphite annulus 1, is poured in cast iron die by supernatant liquid.
Control power to 200kW until silicon ingot is poured out after melting completely.
Embodiment 2:
Install furnace lining 7 and ruhmkorff coil 5 from inside to outside successively in body of heater, plumbago crucible 2 is put in furnace lining 7, water-cooled ingot pulling mechanism 6 is installed bottom plumbago crucible 2, and plumbago crucible 2 and water-cooled ingot pulling mechanism 6 are all in the holding of furnace lining 7.
In plumbago crucible 2, add slag agent total mass is 100kg, first 5kg calcium oxide is added, 5kg silicon-dioxide, the water glass of 5kg Calcium Fluoride (Fluorspan) and 5kg, add 100kg silicon material 4, regulate ruhmkorff coil 5, make heating power be after 300kW to silicon material 4 all fusing, divide and add the agent of residue 80kg slag for 5 times, add melting 30min after slag at every turn, regulate ruhmkorff coil 5, make smelting temperature be 1800 DEG C, then upper strata slag agent 3 is all poured in heat resisting iron mould.
Get and composition in above-mentioned steps and new slag agent 100kg identical in quality, average mark adds in plumbago crucible 5 times, and smelting temperature is 1800 DEG C, upper strata slag agent is all poured in heat resisting iron mould after melting.
Get new slag agent 3 parts, every part of 100kg, every 100kg repeats second step; After melting terminates, last 80kg upper strata slag agent 3 is poured in heat resisting iron mould.
Adjustment plant capacity is 250kW, and controlling smelting temperature is, after 1550 DEG C, carry out preliminary directional freeze.The water-cooled ingot pulling mechanism 6 controlled bottom plumbago crucible 2 pulls down ingot, draws ingot speed to be 6cm/h, and top adds cover graphite annulus 1 simultaneously, and the height of cover graphite annulus 1 is 500mm.Stop drawing ingot when silicon liquid accounts for 20% of silicon material, water-cooled ingot pulling mechanism 6 fast lift velocity is 20cm/min, plumbago crucible 2 is set back, after taking off cover graphite annulus 1, is poured in cast iron die by supernatant liquid.
Control power to 300kW until silicon ingot is poured out after melting completely.
Embodiment 3:
Install furnace lining 7 and ruhmkorff coil 5 from inside to outside successively in body of heater, plumbago crucible 2 is put in furnace lining 7, water-cooled ingot pulling mechanism 6 is installed bottom plumbago crucible 2, and plumbago crucible 2 and water-cooled ingot pulling mechanism 6 are all in the holding of furnace lining 7.
In plumbago crucible 2, add slag agent total mass is 200kg, first 10kg calcium oxide is added, 10kg titanium dioxide, the water glass of 10kg Calcium Fluoride (Fluorspan) and 10kg, add 100kg silicon material 4, regulate ruhmkorff coil 5, make heating power be after 250kW to silicon material 4 all fusing, divide and add the agent of residue 160kg slag for 4 times, add melting 25min after slag at every turn, regulate ruhmkorff coil 5, make smelting temperature be 1700 DEG C, then upper strata slag agent 3 is all poured in heat resisting iron mould.
Get and composition in above-mentioned steps and identical in quality 4 parts of new slag agent every part of 200kg, every 200kg repeats second step, after melting terminates, last 180kg upper strata slag agent 3 is poured in heat resisting iron mould.
Adjustment plant capacity is 200kW, and controlling smelting temperature is, after 1500 DEG C, carry out preliminary directional freeze.The water-cooled ingot pulling mechanism 6 controlled bottom plumbago crucible 2 pulls down ingot, draws ingot speed to be 5cm/h, and top adds cover graphite annulus 1 simultaneously, and the height of cover graphite annulus 1 is 300mm.Stop drawing ingot when silicon liquid accounts for 15% of silicon material, water-cooled ingot pulling mechanism 6 fast lift velocity is 15cm/min, plumbago crucible 2 is set back, after taking off cover graphite annulus 1, is poured in cast iron die by supernatant liquid.
Control power to 250kW until silicon ingot is poured out after melting completely.
To sum up, the integrated artistic time is 15 ~ 20h, and full liquid state is connected boron impurity content in the ingot casting obtained in medium melting and preliminary directional solidification processes and is less than 0.3ppmw; After purifying, ingot casting purity is at more than 4N.Metallic impurity total content is less than 100ppmw.
Claims (8)
1. medium melting is connected a method for purifying polycrystalline silicon with preliminary directional freeze, it is characterized in that, adopts following apparatus to purify:
Plumbago crucible sidewall in body of heater is provided with furnace lining and ruhmkorff coil outward successively, water-cooled ingot pulling mechanism is installed bottom plumbago crucible, and plumbago crucible and water-cooled ingot pulling mechanism are all in furnace lining holds, plumbago crucible top is provided with the cover graphite annulus identical with external diameter size with plumbago crucible internal diameter, and the height of cover graphite annulus is 200 ~ 500mm;
Method of purification comprises silicon material and slag agent to react carries out medium melting, remove the boron impurity in silicon material, after medium melting terminates, the cold ingot pulling mechanism of bottom water is adopted to draw the mode of ingot, preliminary directional freeze is carried out to silicon liquid, gathered by metallic impurity in silicon liquid after top removed, control temperature is poured out after silicon ingot is melted completely.
2. employing medium according to claim 1 melting is connected the method for purifying polycrystalline silicon with preliminary directional freeze, comprises the following steps:
(1) in plumbago crucible, add 10 ~ 20% and whole silicon material of slag agent quality, after control heating power to silicon material all melts, average mark adds the agent of residue slag for 2 ~ 5 times, control ruhmkorff coil, make smelting temperature be 1600 ~ 1800 DEG C, after melting, upper strata slag agent is all poured in heat resisting iron mould;
(2) repeat above-mentioned medium fusion process 1 ~ 3 time, the new slag agent at every turn added divides 2 ~ 5 times and adds;
After it is characterized in that medium melting terminates, be connected following steps:
(3), after melting terminates, pour in heat resisting iron mould by 80 ~ 90% of last slag agent quality;
(4) regulate ruhmkorff coil, make smelting temperature be, after 1450 ~ 1550 DEG C, carry out preliminary directional freeze, the water-cooled ingot pulling mechanism controlled bottom plumbago crucible pulls down ingot, and top adds cover graphite annulus simultaneously; Stop drawing ingot when silicon liquid accounts for 10 ~ 20% of silicon material, the cold ingot pulling mechanism of quick hypogene water, makes plumbago crucible set back, and after taking off cover graphite annulus, is all poured in cast iron die by supernatant liquid;
(5) control power to pour out after silicon ingot melts completely.
3. medium melting according to claim 2 is connected the method for purifying polycrystalline silicon with preliminary directional freeze, and the slag agent that it is characterized in that in step (1) is the mixture of the calcium oxide of arbitrary proportion, Calcium Fluoride (Fluorspan), titanium dioxide, silicon-dioxide and water glass.
4. medium melting according to claim 2 is connected the method for purifying polycrystalline silicon with preliminary directional freeze, it is characterized in that the ratio of slag agent in step (1) and step (2) and silicon material is 1/3 ~ 2/1.
5. medium melting according to claim 2 is connected the method for purifying polycrystalline silicon with preliminary directional freeze, it is characterized in that in step (1) and (5), heating power is 200 ~ 300kW.
6. medium melting according to claim 2 is connected the method for purifying polycrystalline silicon with preliminary directional freeze, it is characterized in that in step (1) and step (2) add slag at every turn after need melting 20 ~ 30min.
7. medium melting according to claim 2 is connected the method for purifying polycrystalline silicon with preliminary directional freeze, it is characterized in that, in step (4), plant capacity is 150 ~ 250kW.
8. medium melting according to claim 2 is connected the method for purifying polycrystalline silicon with preliminary directional freeze, it is characterized in that in step (4), what water-cooled ingot pulling mechanism was downward draws ingot speed to be 4 ~ 6cm/h, and the speed of the cold ingot pulling mechanism of quick hypogene water is 10 ~ 20cm/min.
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| CN109536744B (en) * | 2017-09-22 | 2021-05-04 | 有研稀土新材料股份有限公司 | Method for purifying rare earth metal by liquation directional solidification coupling |
| CN108328618B (en) * | 2018-01-30 | 2021-02-09 | 青岛蓝光晶科新材料有限公司 | Method for separating hard inclusions in silicon by electromagnetic induction directional solidification |
| CN108796606B (en) * | 2018-07-07 | 2020-11-03 | 玉环市几偶孵化器有限公司 | Solar-grade polycrystalline silicon preparation device |
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| CN102849743A (en) * | 2012-09-25 | 2013-01-02 | 青岛隆盛晶硅科技有限公司 | Polysilicon purification method and device by reverse induced solidification |
| CN103072997A (en) * | 2013-02-04 | 2013-05-01 | 福建兴朝阳硅材料股份有限公司 | Method and device for removing metal impurities in polycrystalline silicon |
| CN203568855U (en) * | 2013-10-18 | 2014-04-30 | 青岛隆盛晶硅科技有限公司 | Device for purifying polycrystalline silicon via linkage of medium smelting and primary directional solidification |
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| CN102849743A (en) * | 2012-09-25 | 2013-01-02 | 青岛隆盛晶硅科技有限公司 | Polysilicon purification method and device by reverse induced solidification |
| CN103072997A (en) * | 2013-02-04 | 2013-05-01 | 福建兴朝阳硅材料股份有限公司 | Method and device for removing metal impurities in polycrystalline silicon |
| CN203568855U (en) * | 2013-10-18 | 2014-04-30 | 青岛隆盛晶硅科技有限公司 | Device for purifying polycrystalline silicon via linkage of medium smelting and primary directional solidification |
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