CN103539125A - Device and method for purifying polycrystalline silicon by linking of medium smelting and primary directional solidification - Google Patents
Device and method for purifying polycrystalline silicon by linking of medium smelting and primary directional solidification Download PDFInfo
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Abstract
The invention belongs to the field of polycrystalline silicon purification, and particularly discloses a device and a method for purifying polycrystalline silicon by linking of medium smelting and primary directional solidification. The device is characterized in that the side wall of a graphite crucible in a furnace body is externally successively provided with a furnace lining and an induction coil, and the bottom of the graphite crucible is provided with a water-cooling ingot pulling mechanism; the graphite crucible and the water-cooling ingot pulling mechanism are wrapped in the furnace lining, and the top of the graphite crucible is provided with a graphite filling ring the inner and outer diameters of which are same with the inner and outer diameters of the graphite crucible. The method comprises the following steps that a silicon material reacts with a residue agent for medium smelting to remove boron impurities in the silicon material, after the medium smelting is finished, primary directional solidification is carried out on the silicon liquid by adopting a manner of pulling an ingot by the water-cooling ingot pulling mechanism arranged on the bottom of the device, so that metal impurities in the silicon liquid are gathered to the top so as to be removed, and the temperature is controlled so that a silicon ingot is fully melted so as to be poured. The device and the method provided by the invention have the advantages that full liquid state linking of medium smelting and primary directional solidification is adopted, so that the power consumption is reduced by 1000-2000 kilowatt-hours/ton, the production cost is reduced by 4000-8000 yuan/ton, the content of boron impurities in a cast ingot is less than 0.3ppmw, and the total content of the metal impurities is less than 100ppmw.
Description
Technical field
The invention belongs to polycrystalline silicon purifying field, be specifically related to a kind of medium melting and be connected the device and method of purifying polycrystalline silicon 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 requiring 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 meet completely the needs of modern society.Until the discovery of photoresistance, the manufacture of solar cell, people find sun power new utilize mode.Silicon is as the desirable feedstock of solar cell, impurity wherein mainly contains the nonmetallic impuritys such as the metallic impurity such as Fe, Al, Ca and B, P, 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 has determined the photoelectric transformation efficiency of solar cell, so effectively remove these impurity, in the application aspect of solar cell, there is vital effect.
The development of photovoltaic industry depends on the purification to silicon raw material, in the process of metallurgy method purifying polycrystalline silicon, comprises that medium melting, directional freeze, electron beam purify and casting ingot process.Metallurgy method has development potentiality because possessing simple, the lower-cost advantage of technique.In all multi-steps, with medium melting, require equipment the simplest, the easiest industrialization promotion.Thereby researching value and the application prospect of the tool reality of medium melting.
In traditional medium fusion process, medium melting is the technique that twice are different with directional freeze, removes respectively boron and other metallic impurity.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 need to excise the impurity enriched district on top approximately 20%.In conventional production, understand through supersolidification---fusing---process of resolidification between twice technique, need to consume amount of heat during this, 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 and is connected the device and method of purifying polycrystalline silicon with preliminary directional freeze, in separate unit medium-frequency induction furnace, realizing medium melting is connected with the full liquid state of preliminary directional solidification processes, when removing boron impurity, can remove most of metallic impurity, make silicon material reach 4N level, greatly alleviate the purification pressure of subsequent technique, without integral body is all completed to directional freeze process, silicon is partly poured out impurity enriched under liquid state, the tailing saving after solidifying is removed process, realize directly obtaining of the low borosilicate material of 4N.
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, in plumbago crucible bottom, water-cooled water-cooled ingot pulling mechanism is installed, and plumbago crucible and water-cooled ingot pulling mechanism are all in furnace lining holds, and 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 is reacted and carries out medium melting with slag agent, remove the boron impurity in silicon material, after medium melting finishes, the mode that adopts the cold ingot pulling mechanism of bottom water to draw ingot, silicon liquid is carried out to preliminary directional freeze, after the metallic impurity in silicon liquid are gathered to top and removed, control after temperature melts silicon ingot completely and pour out.
Preferably include following steps:
(1) to 10～20% and the whole silicon material that add slag agent quality in plumbago crucible, control heating power to the whole fusings of silicon material, average mark adds the agent of residue slag for 2～5 times, control ruhmkorff coil, making smelting temperature is 1600～1800 ℃, 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 adding divides 2～5 times and adds;
(3), after melting finishes, by 80～90% of last slag agent quality, pour in heat resisting iron mould;
(4) regulate ruhmkorff coil, after making smelting temperature be 1450～1550 ℃, carry out preliminary directional freeze, the water-cooled ingot pulling mechanism of controlling plumbago crucible bottom pulls down ingot, and top adds cover graphite annulus simultaneously; When silicon liquid account for silicon material 10～20% time stop drawing ingot, fast rise water-cooled ingot pulling mechanism, sets back plumbago crucible, takes off after cover graphite annulus, and supernatant liquid is all poured in cast iron die;
(5) power ratio control is poured out after silicon ingot melts completely.
Preferred version is as follows:
The mixture of calcium oxide, Calcium Fluoride (Fluorspan), titanium dioxide, silicon-dioxide and water glass that the slag agent in step (1) is arbitrary proportion.
Slag agent in step (1) and step (2) and the ratio of silicon material are 1/3～2/1.
In step (1) and (5), heating power is 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), the ingot speed of drawing that water-cooled ingot pulling mechanism is downward is 4～6cm/h, and the speed of fast rise water-cooled ingot pulling mechanism is 10～20cm/min.
Preliminary directional freeze of the present invention is different from the directional freeze in normal process, and the one, need under vacuum condition, not carry out, not high to equipment requirements degree; The 2nd, less demanding to removal of impurities, only need to do preliminary removal to metallic impurity, in remaining silicon ingot, still retain a part of metallic impurity.
In this device, furnace lining is to consist of refractory mortar, and its plasticity-is good, and refractoriness is high, bonding strength is high, and stable chemical nature.The furnace lining lengthening makes water-cooled ingot pulling mechanism drive plumbago crucible to move up and down in furnace lining inside, draw ingot after plumbago crucible move down, add cover graphite annulus, after preventing that plumbago crucible from moving down, the refractory masses exposing is heated and excessive empty burning, reduces equipment loss.In medium melting, add for the first time slag and first add 10～20% of slag agent quality, and then to add silicon material, effect be in order to protect plumbago crucible.When silicon liquid account for silicon material 10～20% time stop drawing ingot, fast rise water-cooled ingot pulling mechanism, plumbago crucible is set back, take off after cover graphite annulus, supernatant liquid is poured in cast iron die, in 10～20% the silicon liquid on this upper strata, impurity enriched degree is higher, treatment process is before after silicon material is all solidified, the silicon material of impurity is rich on excision upper strata, but adopt apparatus of the present invention and method, reduced the step of all solidifying rear excision, directly supernatant liquid is poured out, reduced current consumption, production cost also reduces greatly., the slag agent of pouring out in operation is collected in cast iron die meanwhile, can be for melting again.
The invention has the advantages that: complete liquid medium melting and the preliminary directional solidification processes of being connected, save 1000～2000 KWhs/ton of power consumptions; 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 more than 4N.Metallic impurity total content is less than 100ppmw.Accompanying drawing explanation
Fig. 1 is that medium melting is used schematic diagram with the device that preliminary directional freeze is connected purifying polycrystalline silicon.
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
Below in conjunction with embodiment, describe the present invention in detail, but the present invention is not limited to specific embodiment.
Embodiment 1:
In body of heater, install successively from inside to outside furnace lining 7 and ruhmkorff coil 5, plumbago crucible 2 is put in furnace lining 7, in plumbago crucible 2 bottoms, water-cooled ingot pulling mechanism 6 is installed, and plumbago crucible 2 and water-cooled ingot pulling mechanism 6 are all in the holding of furnace lining 7.
To adding slag agent total mass in plumbago crucible 2, be 50kg, first add 2kg titanium dioxide, 2kg silicon-dioxide, the water glass of 2kg Calcium Fluoride (Fluorspan) and 4kg, add 100kg silicon material 4, regulate ruhmkorff coil 5, making heating power is after 200kW all melts to silicon material 4, divides and adds the agent of residue 40kg slag for 2 times, add melting 20min after slag at every turn, regulate ruhmkorff coil 5, making smelting temperature is 1800 ℃, then upper strata slag agent 3 is all poured in heat resisting iron mould.
Get with above-mentioned steps in composition and new slag agent 50kg identical in quality, average mark adds in plumbago crucible for 2 times, smelting temperature is 1600 ℃, after melting, upper strata slag agent is all poured in heat resisting iron mould.
Get 1 part of the new slag agent of 50kg, repeat second step once; After melting finishes, 40kg upper strata slag agent 3 is poured in heat resisting iron mould.
Adjustment plant capacity is 150kW, after control smelting temperature is 1450 ℃, carries out preliminary directional freeze.The water-cooled ingot pulling mechanism 6 of controlling plumbago crucible 2 bottoms pulls down ingot, and drawing ingot speed is 4cm/h, and top adds cover graphite annulus 1 simultaneously, and the height of cover graphite annulus 1 is 200mm.When silicon liquid account for silicon material 10% time stop drawing ingot, water-cooled ingot pulling mechanism 6 fast rise speed are 10cm/min, and plumbago crucible 2 is set back, and take off after cover graphite annulus 1, and supernatant liquid is poured in cast iron die.
Power ratio control to 200kW until silicon ingot after melting completely, pour out.
Embodiment 2:
In body of heater, install successively from inside to outside furnace lining 7 and ruhmkorff coil 5, plumbago crucible 2 is put in furnace lining 7, in plumbago crucible 2 bottoms, water-cooled ingot pulling mechanism 6 is installed, and plumbago crucible 2 and water-cooled ingot pulling mechanism 6 are all in the holding of furnace lining 7.
To adding slag agent total mass in plumbago crucible 2, be 100kg, first add 5kg calcium oxide, 5kg silicon-dioxide, the water glass of 5kg Calcium Fluoride (Fluorspan) and 5kg, add 100kg silicon material 4, regulate ruhmkorff coil 5, making heating power is after 300kW all melts to silicon material 4, divides and adds the agent of residue 80kg slag for 5 times, add melting 30min after slag at every turn, regulate ruhmkorff coil 5, making smelting temperature is 1800 ℃, then upper strata slag agent 3 is all poured in heat resisting iron mould.
Get with above-mentioned steps in composition and new slag agent 100kg identical in quality, average mark adds in plumbago crucible for 5 times, smelting temperature is 1800 ℃, after melting, upper strata slag agent is all poured in heat resisting iron mould.
Get 3 parts of new slag agent, every part of 100kg, every 100kg repeats second step; After melting finishes, last 80kg upper strata slag agent 3 is poured in heat resisting iron mould.
Adjustment plant capacity is 250kW, after control smelting temperature is 1550 ℃, carries out preliminary directional freeze.The water-cooled ingot pulling mechanism 6 of controlling plumbago crucible 2 bottoms pulls down ingot, and drawing ingot speed is 6cm/h, and top adds cover graphite annulus 1 simultaneously, and the height of cover graphite annulus 1 is 500mm.When silicon liquid account for silicon material 20% time stop drawing ingot, water-cooled ingot pulling mechanism 6 fast rise speed are 20cm/min, and plumbago crucible 2 is set back, and take off after cover graphite annulus 1, and supernatant liquid is poured in cast iron die.
Power ratio control to 300kW until silicon ingot after melting completely, pour out.
Embodiment 3:
In body of heater, install successively from inside to outside furnace lining 7 and ruhmkorff coil 5, plumbago crucible 2 is put in furnace lining 7, in plumbago crucible 2 bottoms, water-cooled ingot pulling mechanism 6 is installed, and plumbago crucible 2 and water-cooled ingot pulling mechanism 6 are all in the holding of furnace lining 7.
To adding slag agent total mass in plumbago crucible 2, be 200kg, first add 10kg calcium oxide, 10kg titanium dioxide, the water glass of 10kg Calcium Fluoride (Fluorspan) and 10kg, add 100kg silicon material 4, regulate ruhmkorff coil 5, making heating power is after 250kW all melts to silicon material 4, divides and adds the agent of residue 160kg slag for 4 times, add melting 25min after slag at every turn, regulate ruhmkorff coil 5, making smelting temperature is 1700 ℃, then upper strata slag agent 3 is all poured in heat resisting iron mould.
Get with above-mentioned steps in composition and 4 parts of new every part of 200kg of slag agent identical in quality, every 200kg repeats second step, after melting finishes, last 180kg upper strata slag agent 3 is poured in heat resisting iron mould.
Adjustment plant capacity is 200kW, after control smelting temperature is 1500 ℃, carries out preliminary directional freeze.The water-cooled ingot pulling mechanism 6 of controlling plumbago crucible 2 bottoms pulls down ingot, and drawing ingot speed is 5cm/h, and top adds cover graphite annulus 1 simultaneously, and the height of cover graphite annulus 1 is 300mm.When silicon liquid account for silicon material 15% time stop drawing ingot, water-cooled ingot pulling mechanism 6 fast rise speed are 15cm/min, and plumbago crucible 2 is set back, and take off after cover graphite annulus 1, and supernatant liquid is poured in cast iron die.
Power ratio control to 250kW until silicon ingot after melting completely, pour out.
To sum up, the integrated artistic time is 15～20h, and in the ingot casting obtaining in complete liquid linking medium melting and preliminary directional solidification processes, boron impurity content is less than 0.3ppmw; After purifying, ingot casting purity is more than 4N.Metallic impurity total content is less than 100ppmw.
Claims (10)
1. a medium melting 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, it is characterized in that, in plumbago crucible bottom, water-cooled ingot pulling mechanism is installed, and plumbago crucible and water-cooled ingot pulling mechanism are all in furnace lining holds, and plumbago crucible top is provided with the cover graphite annulus identical with external diameter size with plumbago crucible internal diameter.
2. medium melting according to claim 1 is connected the device of purifying polycrystalline silicon with preliminary directional freeze, and the height that it is characterized in that cover graphite annulus is 200～500mm.
3. one kind adopts medium melting claimed in claim 1 to be connected the method for the device of purifying polycrystalline silicon with preliminary directional freeze, comprise silicon material is reacted and carries out medium melting with slag agent, remove the boron impurity in silicon material, after it is characterized in that medium melting finishes, the mode that adopts the cold ingot pulling mechanism of bottom water to draw ingot, silicon liquid is carried out to preliminary directional freeze, after the metallic impurity in silicon liquid are gathered to top and removed, control after temperature melts silicon ingot completely and pour out.
4. medium melting according to claim 3 is connected the method for the device of purifying polycrystalline silicon with preliminary directional freeze, comprises the following steps:
(1) to 10～20% and the whole silicon material that add slag agent quality in plumbago crucible, control heating power to the whole fusings of silicon material, average mark adds the agent of residue slag for 2～5 times, control ruhmkorff coil, making smelting temperature is 1600～1800 ℃, 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 adding divides 2～5 times and adds;
After it is characterized in that medium melting finishes, be connected following steps:
(3), after melting finishes, by 80～90% of last slag agent quality, pour in heat resisting iron mould;
(4) regulate ruhmkorff coil, after making smelting temperature be 1450～1550 ℃, carry out preliminary directional freeze, the water-cooled ingot pulling mechanism of controlling plumbago crucible bottom pulls down ingot, and top adds cover graphite annulus simultaneously; When silicon liquid account for silicon material 10～20% time stop drawing ingot, fast rise water-cooled ingot pulling mechanism, sets back plumbago crucible, takes off after cover graphite annulus, and supernatant liquid is all poured in cast iron die;
(5) power ratio control is poured out after silicon ingot melts completely.
5. medium melting according to claim 3 is connected the method for purifying polycrystalline silicon with preliminary directional freeze, it is characterized in that the mixture of calcium oxide, Calcium Fluoride (Fluorspan), titanium dioxide, silicon-dioxide and water glass that the slag agent in step (1) is arbitrary proportion.
6. medium melting according to claim 3 is connected the method for purifying polycrystalline silicon with preliminary directional freeze, it is characterized in that slag agent in step (1) and step (2) and the ratio of silicon material are 1/3～2/1.
7. medium melting according to claim 3 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.
8. medium melting according to claim 3 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.
9. medium melting according to claim 3 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.
10. medium melting according to claim 3 is connected the method for purifying polycrystalline silicon with preliminary directional freeze, it is characterized in that in step (4), the ingot speed of drawing that water-cooled ingot pulling mechanism is downward is 4～6cm/h, and the speed of fast rise water-cooled ingot pulling mechanism is 10～20cm/min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108328618A (en) * | 2018-01-30 | 2018-07-27 | 青岛蓝光晶科新材料有限公司 | A kind of method of hard inclusions in electromagnetic induction directional solidification divided silicon |
| CN108796606A (en) * | 2018-07-07 | 2018-11-13 | 孟静 | Solar-grade polysilicon preparation facilities |
| CN109536744A (en) * | 2017-09-22 | 2019-03-29 | 有研稀土新材料股份有限公司 | The method for coupling Purification of Rare Earth Metals by liquate 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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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109536744A (en) * | 2017-09-22 | 2019-03-29 | 有研稀土新材料股份有限公司 | The method for coupling Purification of Rare Earth Metals by liquate directional solidification |
| CN108328618A (en) * | 2018-01-30 | 2018-07-27 | 青岛蓝光晶科新材料有限公司 | A kind of method of hard inclusions in electromagnetic induction directional solidification divided silicon |
| 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 |
| CN108796606A (en) * | 2018-07-07 | 2018-11-13 | 孟静 | Solar-grade polysilicon preparation facilities |
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