CN203568855U - Device for purifying polycrystalline silicon via linkage of medium smelting and primary directional solidification - Google Patents
Device for purifying polycrystalline silicon via linkage of medium smelting and primary directional solidification Download PDFInfo
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- CN203568855U CN203568855U CN201320646244.8U CN201320646244U CN203568855U CN 203568855 U CN203568855 U CN 203568855U CN 201320646244 U CN201320646244 U CN 201320646244U CN 203568855 U CN203568855 U CN 203568855U
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- polycrystalline silicon
- plumbago crucible
- graphite crucible
- pulling mechanism
- ingot
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- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 11
- 238000003723 Smelting Methods 0.000 title abstract description 12
- 238000007711 solidification Methods 0.000 title abstract description 7
- 230000008023 solidification Effects 0.000 title abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 51
- 239000010439 graphite Substances 0.000 claims abstract description 50
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 19
- 241000209456 Plumbago Species 0.000 claims description 31
- 230000008018 melting Effects 0.000 claims description 24
- 238000002844 melting Methods 0.000 claims description 24
- 239000012535 impurity Substances 0.000 abstract description 18
- 238000000034 method Methods 0.000 abstract description 17
- 239000007788 liquid Substances 0.000 abstract description 11
- 229910052796 boron Inorganic materials 0.000 abstract description 6
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000000746 purification Methods 0.000 abstract description 3
- 230000006698 induction Effects 0.000 abstract description 2
- 238000001816 cooling Methods 0.000 abstract 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 2
- 230000005611 electricity Effects 0.000 abstract 1
- 239000002184 metal Substances 0.000 abstract 1
- 239000002893 slag Substances 0.000 description 22
- 239000003795 chemical substances by application Substances 0.000 description 20
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 17
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 12
- 229910052710 silicon Inorganic materials 0.000 description 12
- 239000010703 silicon Substances 0.000 description 12
- 239000002210 silicon-based material Substances 0.000 description 11
- 229910052742 iron Inorganic materials 0.000 description 9
- 238000005266 casting Methods 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 229910001018 Cast iron Inorganic materials 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 2
- 229910001634 calcium fluoride Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000007499 fusion processing Methods 0.000 description 2
- 238000005272 metallurgy Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 235000019353 potassium silicate Nutrition 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 229960001866 silicon dioxide Drugs 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 1
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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- Silicon Compounds (AREA)
Abstract
The utility model relates to a device for purifying polycrystalline silicon via linkage of medium smelting and primary directional solidification, and belongs to the field of purification of polycrystalline silicon. The device is characterized in that a furnace lining and an induction coil are sequentially mounted outside the sidewall of a graphite crucible in a furnace body; a water cooling ingot pulling mechanism is mounted at the bottom part of the graphite crucible; both the graphite crucible and the water cooling ingot pulling mechanism are surrounded with the furnace lining; a coverage graphite ring, of which the inside diameter and outside diameter are the same as those of the graphite crucible, is mounted on the top part of the graphite crucible. The device has the advantages that the medium smelting process and the primary directional solidification process are linked in a full-liquid state, and thus the electricity consumption can be saved by 1,000 to 2,000KWh per ton, and the cost of production by medium smelting is also reduced by 4,000 to 8,000 Yuan per ton; a cast ingot contains less than 0.3ppmw of boron impurity; the purified cast ingot has the purity exceeding 4N; the total metal impurity content is less than 100ppmw.
Description
Technical field
The utility model belongs to polycrystalline silicon purifying field, is specifically related to a kind of medium melting and is connected the device 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.
Utility model content
According to above the deficiencies in the prior art, the utility model proposes a kind of medium melting and be connected the device 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 described in the utility model 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 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.
The operation steps of this device is as follows:
(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, regulate ruhmkorff coil, controlling 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 control smelting temperature is 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.
Described preliminary directional freeze 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.
The utility model has the advantage of: adopt this device liquid medium melting and preliminary directional solidification processes of being connected entirely, 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 use schematic diagram of the present utility model.
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 utility model in detail, but the utility model 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, adds 100kg silicon material 4, regulate ruhmkorff coil 5, control heating power and be 200kW to silicon material 4 all after fusing, minute add the agent of residue 40kg slag for 2 times, add melting 20min after slag at every turn, 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, adds 100kg silicon material 4, regulate ruhmkorff coil 5, control heating power and be 300kW to silicon material 4 all after fusing, minute add the agent of residue 80kg slag for 5 times, add melting 30min after slag at every turn, 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.
To sum up, adopt this device, 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 (2)
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.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201320646244.8U CN203568855U (en) | 2013-10-18 | 2013-10-18 | Device for purifying polycrystalline silicon via linkage of medium smelting and primary directional solidification |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201320646244.8U CN203568855U (en) | 2013-10-18 | 2013-10-18 | Device for purifying polycrystalline silicon via linkage of medium smelting and primary directional solidification |
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| CN203568855U true CN203568855U (en) | 2014-04-30 |
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| CN201320646244.8U Expired - Fee Related CN203568855U (en) | 2013-10-18 | 2013-10-18 | Device for purifying polycrystalline silicon via linkage of medium smelting and primary directional solidification |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103539125A (en) * | 2013-10-18 | 2014-01-29 | 青岛隆盛晶硅科技有限公司 | Device and method for purifying polycrystalline silicon by linking of medium smelting and primary directional solidification |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103539125A (en) * | 2013-10-18 | 2014-01-29 | 青岛隆盛晶硅科技有限公司 | Device and method for purifying polycrystalline silicon by linking of medium smelting and primary directional solidification |
| CN103539125B (en) * | 2013-10-18 | 2015-09-02 | 青岛隆盛晶硅科技有限公司 | Medium melting is connected the method for purifying polycrystalline silicon with preliminary directional freeze |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20171117 Address after: 1 road 266000 in Shandong province Qingdao city Laoshan District No. 1 Keyuan latitude B block 7 layer B4-2 Patentee after: Qingdao Changsheng Dongfang Industry Group Co., Ltd. Address before: Pudong solar energy industry base in Jimo city of Shandong Province, Qingdao City, 266234 Patentee before: Qingdao Longsheng Crystalline Silicon Science & Technology Co., Ltd. |
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| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20171124 Address after: Miao road Laoshan District 266061 Shandong city of Qingdao Province, No. 52 906 Patentee after: Qingdao Changsheng Electric Design Institute Co. Ltd. Address before: 1 road 266000 in Shandong province Qingdao city Laoshan District No. 1 Keyuan latitude B block 7 layer B4-2 Patentee before: Qingdao Changsheng Dongfang Industry Group Co., Ltd. |
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| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20140430 Termination date: 20191018 |