CN101585536B - Device and method for purifying solar energy level polysilicon - Google Patents

Device and method for purifying solar energy level polysilicon Download PDF

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CN101585536B
CN101585536B CN200910304025XA CN200910304025A CN101585536B CN 101585536 B CN101585536 B CN 101585536B CN 200910304025X A CN200910304025X A CN 200910304025XA CN 200910304025 A CN200910304025 A CN 200910304025A CN 101585536 B CN101585536 B CN 101585536B
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furnace
electron
silicon
district
unidirectional solidification
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CN101585536A (en
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李廷举
刘宏伟
张国梁
刘勤煜
张剑
马红军
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Dalian University of Technology
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Dalian University of Technology
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Abstract

The present invention discloses a device and a method for purifying solar energy level polysilicon, belonging to a technology field for preparing a kind of novel energy source material. The method includes steps: comminuting the industrial silicon firstly and removing predominant metallic impurity elements from the industrial silicon with exposed surface by an ultrasound and gas agitation picklingtreatment; purifying further by vacuum induction smelting, three-zone temperature-controlled semi-continuous unidirectional solidification, high vacuum electronic torch melting and secondary three-zo ne temperature-controlled semi-continuous unidirectional solidification; finally obtaining a polysilicon casting ingot with an uniform column-shaped solidification organization. The method and the device of the invention have advantages of stabile technique, low cost, non pollution, convenient equipment operation, etc.; the prepared polysilicon casting ingot has an uniform structure, non flaw and non air sac, and is suitable for preparing a solar battery.

Description

A kind of apparatus and method of purifying solar energy level polysilicon
Technical field
The invention belongs to the new energy materials preparing technical field, relate to a kind of preparation technology and device of used for solar batteries high purity polycrystalline silicon.
Background technology
Solar cell industry receives the common concern of each country of the whole world as the main strategic energy industry in future.But as emerging scientific and technological industry, current technical superiority still remains in the minority advanced country hands such as Japan, Germany and the U.S..Present photovoltaic product about 90% is still based on crystal silicon battery, and polycrystalline silicon solar cell accounts for 52.3% of the solar cell market share.The production of whole world crystalline silicon is mainly grasped in Hemlock, Tokuyama, Wacker, Asimi, MEMC, Mitsubishi, SGS and Sumitomo eight large manufacturer's hands, and its quality product location almost is electronic-grade polycrystalline silicon, and main production method is chemical processes such as improvement Siemens Method, silane thermal decomposition process and fluidized bed method.And, mainly exist with these chemical process production HIGH-PURITY SILICON forms with the form of silicon particle, though purity is very high, do not reach the required ratio resistance of solar cell substrate than resistance and require (0.5~1.5 lonely cm), therefore can't be directly used in and make the solar cell substrate.Need fusion again, carry out adopting the method for pulling monocrystal or polycrystalline directional freeze to form silicon ingot, microsection manufacture solar cell substrate then after composition adjusts.
The upstream raw material of present traditional crystal silicon photovoltaic battery mainly relies on the leftover bits and the residue production capacity of semi-conductor industry.And in recent years photovoltaic industry grow continuously and fast and semi-conductor industry begins to recover gradually and causes the in short supply of upstream silicon material, cause solar-grade polysilicon price one tunnel surging, to the highest 300~400 dollars/kilogram, seriously restricted the development of the world (especially China) photovoltaic industry by 60 dollars/kilogram in 2000.For satisfying the demand to 6N purity polysilicon of solar cell, various novel procesies are being developed in the whole world energetically.
For example, blink Wan CS and hydrogen of the Ji LD Yi ひ of the public department of Tokuyama enters the carbon tube that is heated to 1500 ℃ from the upper end, and the silicon that restores is cooled to granular with liquid state deposition drippage; The TCS-FBR reactor SiHCl of Wacker company 3+ H 2Reduction method; The FBR reactor SiH of SGS/Asimi company 4Thermal decomposition method; Jssi company replaces the silicon core to be the SiH of carrier with silicone tube 4Thermal decomposition method is produced powdery silicon, and compression moulding is used then; Gti company replaces many SiHCl that make carrier (heating element) of the silicon core with silicone tube 3+ H 2Reduction (decomposition) method; The employing SiCl that Chisso company carries out 4Zinc reduction research; Also has the hot carbon reduction technology of silica of ECN company etc.But owing to some reasons, these methods mostly are in laboratory or pilot scale stage.
Except that above some progress based on chemical process, researching and developing energetically of various countries adopts the physical metallurgy method to prepare solar-grade polysilicon.
For example, Chinese patent 200710012825.5, a kind of method for manufacturing polycrystalline silicon used for solar battery, with chemical pure industrial silicon and the synthetic SiO of glass sand, utilize SiO disproportionation reaction, acid dipping separation then, in copper crucible, carry out prepared 6N used for solar batteries high purity polycrystalline silicons such as vacuum electron beam melting, plasma melting and directional freeze earlier.Chinese patent 96198989.0, the manufacture method of the manufacturing method and apparatus of polysilicon and silicon for solar cell substrate, the refining of earlier Pure Silicon Metal being reduced pressure in copper crucible or plumbago crucible is again in H 2O, CO 2Or O 2Remove carbon and boron in the oxidizing atmosphere that forms, then plasma body winding-up Ar 2, or Ar 2And H 2Mixture carry out deoxidation, obtain ingot casting through directional freeze then,
Chinese patent 200610017755, P type solar cell grade polycrystalline silicon preparing process, with the higher-grade silica is raw material, mixture reduction silica with high-purity refinery coke and coal, then through intermediate frequency (IF) smelting, centrifugal removal of impurities, vibration removal of impurities, two-layer silicon water curtain be set in equipment carry out electron beam dephosphorization, ingot casting, obtain the P type polysilicon of 6~7N.This patent needs to be lower than 100ppmw with single metal content of planting, and the silica that total metal contents in soil is lower than 3000ppmw is a raw material.
Chinese patent ZL02135841.9, produce the method for high-purity silicon for solar energy cell, the addition material that lime, ferric oxide and fluorite are formed is added in employing in molten metal silicon, aerating oxygen, chlorine or steam-laden hydrogen are removed impurity then, carry out directional freeze with the setting rate of 20 ~ 10mm/h in crystallizer at last and obtain 3~5N polysilicon.Chinese patent ZL200310105314.X, a kind of production unit of silicon for solar cell and method adopt Medium frequency induction melting and plasma melting Pure Silicon Metal, add refining slag then, pour into then in the mold, and cooling obtains polycrystalline silicon ingot casting.People such as the Takashi Ikeda of Tokyo Univ Japan also propose to utilize electron beam purifying polycrystalline silicon technology.Kawasaki, Japan system iron (JFE) has been set up a demo plant under the support of NEDO (NewEnergy Development Organization), its technology is removed P at first adopting the vacuum electron beam melting, removes Al and Fe by a directional freeze; In plasma furnace,, make solar-grade polysilicon by the secondary directional freeze more then by removing B with argon plasma and steam reaction. still, it is carrier that these methods all directly adopt plumbago crucible.
Chinese patent 200610134107.0, a kind of production method of solar-grade polysilicon at first graphite or carbon black or the vacuum calcination in 1500~2000 ℃ hot environment of oil glue, is purified; The high purity graphite of glass sand and purification or carbon black or oil glue are added the reduction furnace reduction according to amount of substance than 1: 2, generate the low silicon product of foreign matter content; Again silicon is carried out vacuum fusion in vacuum melting furnace, according to the fusing point controlled temperature of silicon, filter cleaner removes carbon elimination, silicon carbide and silicon dioxide powder impurity, again the silicon of molten state is poured in the mold, directional freeze, get final product the solar-grade polysilicon of 6N level.
A kind of method of removing carbon elimination and metallic impurity from polysilicon surface is proposed among the United States Patent (USP) NO.4525336.Methods such as the processing of employing nitrate aqueous solution, high temperature annealing, the washing of HF burn into are removed the carbon in the polysilicon.Adopt magnetic separation to separate and chemically separated method removal metallic impurity.
Japanese Patent 62-252393 announces a kind of useless silicon that semi-conductor industry is used as starting raw material, uses the plasma jet of the gas mixture generation of argon, hydrogen and oxygen to carry out zone melting, preparation silicon for solar cell ingot.United States Patent (USP) NO.5788945 is also at the waste material of semicon industry, propose a kind of removal wherein boron impurity to satisfy the method for silicon for solar cell requirement.
Summary of the invention
It is starting material with industrial silicon (purity is 99%) that the technical problem to be solved in the present invention provides a kind of, through ultrasonic gas compound pickling, the semicontinuous unidirectional solidification of vacuum induction melting Jia San district temperature control cast, again with the unsettled clamping of the ingot casting that obtains, through technologies such as the semicontinuous unidirectional solidification castings of vacuum electron beam melting Jia San district's temperature control, the technology and the device of preparation polycrystalline silicon used for solar battery ingot casting.
The technical solution adopted in the present invention is:
The particle industrial silicon is placed the pickling pretreatment unit, apply ultrasonic wave from device top respectively,, remove the impurity that silicon grain exposes the crystal boundary place from the bottom of device blowing compressed air; Further refining, purifying industrial silicon directly prepare the solar-grade high-purity polycrystalline silicon ingot casting in semicontinuous unidirectional solidification ingot casting device of vacuum induction melting Jia San district temperature control and the semicontinuous unidirectional solidification ingot casting device of electron beam melting Jia San district temperature control.
Temperature control semicontinuous unidirectional solidification ingot casting device in vacuum induction melting Jia San district involved in the present invention mainly is made of continuous charging device, induction melting furnace, insulation refining furnace, unidirectional solidification low-temperature receiver and towbar He San district temperature controlling system.
But continuous charging device lattice holds silicon material or refining agent, in the induction melting process silicon material is added in the melt.
Induction melting furnace is installed in the ruhmkorff coil by the high-purity silica pot of overcoat plumbago crucible and constitutes, and can realize the fusing of silicon material, induction melting rated output 100kW, supply frequency 1000~2500Hz.
Lay high-purity silica pot in the insulation refining furnace,, carry out refining and solidify in order to hold the silicon melt that melting finishes.The insulation refining furnace is thermal source with the graphite heater, and it is wall that heat preserving and insulating material and stainless steel are adopted in the outside, and inner by high purity graphite and high-purity silica pot isolation, the temperature range of insulation refining furnace is 1450 ~ 1550 ℃.The thermal radiation meeting of graphite heater causes convection current in molten silicon body, can effectively reduce the impurity enriched layer thickness in solid-liquid interface forward position, improves impurity segregation speed.
The material of unidirectional solidification low-temperature receiver and towbar is nonmagnetic stainless steel.Low-temperature receiver and towbar are inner to lead to recirculated cooling water, and links to each other with traction electric machine, can realize the at the uniform velocity decline of ingot casting, and lowering speed can be adjusted between 10~1000mm/h continuously.By the speed of cooling of control unidirectional solidification low-temperature receiver and the lowering speed of towbar, can control the crystalline speed of growth in the melt; With insulation refining furnace compound action, can control solid-liquid interface maintenance flat state in the melt, thereby obtain orthotropic columanar structure.
Three district's temperature controlling systems are made of temperature control unit, last district, temperature control unit, middle district and inferior segment temperature control unit three parts in insulation refining furnace bottom, and controlled temperature range is 600 ~ 1200 ℃.Insulation refining furnace He San district temperature controlling system can accurately be controlled ingot casting week side temperature distribution, realizes multi-region temperature control, gradient cooling in the ingot solidification process; Under the traction of unidirectional solidification towbar, realize the semicontinuous unidirectional solidification of ingot casting.
Temperature control semicontinuous unidirectional solidification ingot casting device in electron beam melting Jia San district involved in the present invention is made of electron beam gun, video observing device, the feed mechanism He San district semicontinuous unidirectional solidification ingot casting device of temperature control.
Electron beam gun is an indirect-heating secondary rifle, can produce high-energy-density beam bombardment silicon material until fusing.But electron beam gun deflection, thereby realize the silicon ingot of unsettled clamping and the silicon melt two station meltings in the crucible.
The video observing device by camera, dodge frequently that mechanism and display screen form, can Real Time Observation and write down silicon ingot and crucible in the melting situation, help the melting technology improvement.
Feed mechanism can be with the unsettled clamping of silicon ingot, and by the predetermined speed charging, the input speed of feed mechanism is that 0 ~ 50mm/min is adjustable continuously.The clamping head adjustable size, in case of necessity can a plurality of ingot castings of clamping to increase the melting amount.
The semicontinuous unidirectional solidification ingot casting device of three district temperature controls in the electron beam furnace comprises insulation refining furnace, unidirectional solidification low-temperature receiver, towbar He San district temperature controlling system, and the interior semicontinuous unidirectional solidification ingot casting device of three district's temperature controls of its function and vacuum induction melting furnace is identical.Electron beam melting and the semicontinuous unidirectional solidification process of three district's temperature controls are realized seamless link, improve refining efficiency.
The solar-grade polysilicon method of purification that the present invention relates to may further comprise the steps:
Step 1: industrial silica fume is broken into particle, is placed on and fills HCl, HNO 3Or carry out cleanup acid treatment in the container of HF, and apply ultrasonic wave from device top respectively, from the bottom of device blowing compressed air, remove the impurity that silicon grain exposes the crystal boundary place; After the processing, be washed till neutrality with deionized water, and oven dry.
Step 2: the industrial silicon particle that will handle is placed in the smelting furnace of vacuum induction melting, and vacuum is evacuated to 10 -2When Pa is above, start the power supply of vacuum induction melting,, make its fusing by ruhmkorff coil heating silicon grain.
Step 3: the silicon melt after the refining is poured into high-purity silica pot in the insulation refining furnace of induction melting furnace, after the insulation refining, strengthen the low-temperature receiver amount of cooling water, crucible is fallen into the temperature controlling system zone, three districts of vacuum induction melting with towbar, carry out the semicontinuous unidirectional solidification of three district's temperature controls, obtain polycrystalline silicon ingot casting.
Step 4: with step 3 gained silicon ingot is raw material, after excision silicon ingot epidermis and the portion end to end, in the unsettled feed mechanism that is clamped in electron beam furnace of residue silicon ingot; Be evacuated to 10 -2~10 -3During Pa, start electron beam gun bombardment silicon ingot, the silicon melt after the fusing directly splashes in the interior high-purity silica pot of insulation refining furnace of electron beam furnace; After silicon ingot melts fully, adjust electron beam gun bombardment silicon melt, carry out refining; After refining finishes, strengthen the low-temperature receiver amount of cooling water, crucible is fallen into the temperature controlling system zone, three districts of electron beam furnace with the towbar of child bundle stove, carries out the semicontinuous unidirectional solidification of three district's temperature controls second time, obtains polycrystalline silicon ingot casting.
Step 5: but repeating step four operations once obtain the used for solar batteries high purity polycrystalline silicon of purity at 6N in case of necessity.
Effect of the present invention and benefit are to reduce used for solar batteries high purity polycrystalline silicon low cost, avoid environmental pollution.
Description of drawings
Fig. 1 is the semicontinuous unidirectional solidification ingot casting device of vacuum induction melting Jia San district temperature control.
Fig. 2 is the semicontinuous unidirectional solidification ingot casting device of electron beam melting Jia San district temperature control.
Among the figure: 1 continuous charging device; 2 induction melting furnaces; 3 silicon melts; The high-purity silica pot of 4 insulation refining furnaces; The insulation refining furnace of 5 vacuum induction furnaces; The silicon melt of 6 insulation refining furnaces; The unidirectional solidification low-temperature receiver of 7 vacuum induction furnaces; The towbar of 8 vacuum induction furnaces; Three district's temperature controlling systems of 9 vacuum induction furnaces; 10 electron beam gun; 11 video observing devices; 12 silicon ingots; 13 feed mechanisms; The insulation refining furnace of 14 electron beam furnaces; The high-purity silica pot of 15 electron beam furnaces; The silicon melt of 16 electron beam furnaces; The unidirectional solidification low-temperature receiver of 17 electron beam furnaces; The towbar of 18 electron beam furnaces; Three district's temperature controlling systems of 19 electron beam furnaces.
Embodiment
Describe specific embodiments of the invention in detail below in conjunction with technical scheme and accompanying drawing.
Embodiment 1
After industrial silicon is broken for 50 ~ 100 order silicon grains, after magnetic force screening, acetone and washed with de-ionized water, be immersed in 50 ℃ the HCl solution, and apply the ultrasonic wave of 20kHz, 80W, feed the air of 6MPa simultaneously, handle after 8 hours extremely neutral with deionized water wash; The oven dry of the silicon grain handled is put into the high-purity silica pot of overcoat plumbago crucible after 300 ℃ by continuous charging device 1, by induction melting furnace 2 heating, after the fusing silicon melt 3 is poured in the high-purity silica pot 4 of insulation refining furnace, 1450 ℃ of insulations 30 minutes, unidirectional solidification low-temperature receiver 7 cooling water flows of vacuum induction furnace remain 500L/h, the high-purity silica pot 4 of insulation refining furnace is fallen into three district's temperature controlling systems, 9 zones of vacuum induction furnace with the towbar 8 of vacuum induction furnace, carry out the semicontinuous unidirectional solidification of three district's temperature controls, setting rate is 3mm/min, obtains the unidirectional solidification silicon ingot of diameter 120mm.
With 12 excisions of the silicon ingot that makes end to end with exterior skin after, utilize feed mechanism 13 clampings, under high vacuum condition by electron beam gun 10 fusings, directly splash in the high-purity silica pot 15 of electron beam furnace, refining 30 minutes, and, impurity element is fully volatilized 1450 ℃ of insulations 1 hour.The speed of feed of feed mechanism 13 is 2mm/min; Strengthen unidirectional solidification low-temperature receiver 17 amount of cooling water of electron beam furnace, the high-purity silica pot 15 of electron beam furnace is fallen into three district's temperature controlling systems, 19 zones of electron beam furnace with the towbar 18 of electron beam furnace, carry out the semicontinuous unidirectional solidification of three district's temperature controls second time, setting rate is 2mm/min, makes the polycrystalline silicon ingot casting of diameter 100mm.By analysis, polycrystalline silicon ingot casting has orthotropic, thick column crystal, and its purity is more than the 5N.
Embodiment 2
After industrial silicon is broken for 50~100 order silicon grains, after magnetic force screening, acetone and washed with de-ionized water, be immersed in 50 ℃ the HCl solution, and apply the ultrasonic wave of 20kHz, 80W, feed the air of 6MPa simultaneously, handle after 24 hours extremely neutral with deionized water wash; The oven dry of the silicon grain handled is put into the high-purity silica pot of overcoat plumbago crucible after 300 ℃ by continuous charging device 1, by induction melting furnace 2 heating, after the fusing silicon melt 3 is poured in the high-purity silica pot 4 of insulation refining furnace, 1500 ℃ of insulations 60 minutes, unidirectional solidification low-temperature receiver 7 cooling water flows of vacuum induction furnace remain 300L/h, the high-purity silica pot 4 of insulation refining furnace is fallen into three district's temperature controlling systems, 9 zones of vacuum induction furnace with the towbar 8 of vacuum induction furnace, carry out the semicontinuous unidirectional solidification of three district's temperature controls, setting rate is 2mm/min, obtains the unidirectional solidification silicon ingot of diameter 120mm.
With 12 excisions of the silicon ingot that makes end to end with exterior skin after, utilize feed mechanism 13 clampings, under high vacuum condition by electron beam gun 10 fusings, directly splash in the high-purity silica pot 15 of electron beam furnace, refining 30 minutes, and, impurity element is fully volatilized 1500 ℃ of insulations 1 hour.The speed of feed of feed mechanism 13 is 1.5mm/min; Strengthen unidirectional solidification low-temperature receiver 17 amount of cooling water of electron beam furnace, the high-purity silica pot 15 of electron beam furnace is fallen into three district's temperature controlling systems, 19 zones of electron beam furnace with the towbar 18 of electron beam furnace, carry out the semicontinuous unidirectional solidification of three district's temperature controls second time, setting rate is 1.5mm/min, makes the polycrystalline silicon ingot casting of diameter 100mm.By analysis, polycrystalline silicon ingot casting has orthotropic, thick column crystal, and its purity is more than the 5N.

Claims (2)

1. the device of a purifying solar energy level polysilicon, this device comprises semicontinuous unidirectional solidification ingot casting device of vacuum induction melting Jia San district temperature control and the semicontinuous unidirectional solidification ingot casting device of electron beam melting Jia San district temperature control, it is characterized in that:
Temperature control semicontinuous unidirectional solidification ingot casting device in vacuum induction melting Jia San district mainly is made of the towbar (8) of insulation refining furnace (5), unidirectional solidification low-temperature receiver (7) and the vacuum induction furnace of continuous charging device (1), induction melting furnace (2), vacuum induction furnace and three district's temperature controlling systems (9) of vacuum induction furnace; High-purity silica pot is placed in the insulation refining furnace (5) of vacuum induction furnace; The insulation refining furnace (5) of vacuum induction furnace is thermal source with the graphite heater, and it is wall that heat preserving and insulating material and stainless steel are adopted in the outside, and is inner by high purity graphite and high-purity silica pot isolation; Three district's temperature controlling systems (9) of vacuum induction furnace are made of temperature control unit, last district, temperature control unit, middle district and inferior segment temperature control unit three parts in insulation refining furnace bottom;
The electron beam melting device comprises electron beam gun (10), video observing device (11) and feed mechanism (13) composition; Feed mechanism (13) is the unsettled clamping of silicon ingot (12), and by the predetermined speed charging, and the clamping head adjustable size can a plurality of ingot castings of clamping; Electron beam melting and the seamless link of the semicontinuous unidirectional solidification process of three district's temperature controls.
2. utilize the method for the described device purifying solar energy level polysilicon of claim 1, its feature comprises following steps:
Step 1: industrial silica fume is broken into particle carries out cleanup acid treatment, apply ultrasonic wave from device top respectively, from the bottom of device blowing compressed air, after the removal silicon grain exposes the impurity processing at crystal boundary place, the washing oven dry;
Step 2: the industrial silicon particle that will handle is placed on fusing in the induction melting furnace; The silicon melt of induction melting is poured into the high-purity silica pot that is incubated refining furnace, after the insulation refining, fall into the temperature controlling system zone, three districts of vacuum induction furnace, carry out the semicontinuous unidirectional solidification of three district's temperature controls, obtain polycrystalline silicon ingot casting by the towbar of vacuum induction furnace;
Step 3: with step 2 gained silicon ingot is raw material, after excision silicon ingot epidermis and the portion end to end, in the unsettled feed mechanism that is clamped in electron beam furnace of residue silicon ingot; Be evacuated to 10 -2~10 -3During Pa, start electron beam gun bombardment silicon ingot, the silicon melt after the fusing directly splashes in the high-purity silica pot of electron beam furnace; After silicon ingot melts fully, adjust the silicon melt of electron beam gun bombardment electron beam furnace, carry out refining; After refining finishes, fall into the temperature controlling system zone, three districts of electron beam furnace, carry out the semicontinuous unidirectional solidification of three district's temperature controls second time, obtain polycrystalline silicon ingot casting by the towbar traction of electron beam furnace;
Step 4: repeating step three obtains the used for solar batteries high purity polycrystalline silicon of purity at 6N.
CN200910304025XA 2009-07-04 2009-07-04 Device and method for purifying solar energy level polysilicon Expired - Fee Related CN101585536B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4525336A (en) * 1983-09-08 1985-06-25 Wacker-Chemitronic Gesellschaft Fur Elektronik Grundstoffe M.B.H. Process for removing impurities from silicon fragments
CN1873062A (en) * 2006-05-06 2006-12-06 大连理工大学 Method for preparing polysilicon in high purity in use for solar cell
CN101307487A (en) * 2007-05-16 2008-11-19 佳科太阳能硅(厦门)有限公司 Directional solidification method and its device for continuous production for polycrystalline silicon ingot

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4525336A (en) * 1983-09-08 1985-06-25 Wacker-Chemitronic Gesellschaft Fur Elektronik Grundstoffe M.B.H. Process for removing impurities from silicon fragments
CN1873062A (en) * 2006-05-06 2006-12-06 大连理工大学 Method for preparing polysilicon in high purity in use for solar cell
CN101307487A (en) * 2007-05-16 2008-11-19 佳科太阳能硅(厦门)有限公司 Directional solidification method and its device for continuous production for polycrystalline silicon ingot

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