CN101824650A - Purifying system of high purity polysilicon and purifying method - Google Patents
Purifying system of high purity polysilicon and purifying method Download PDFInfo
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Abstract
The invention discloses a purifying system of high purity polysilicon and a method for preparing the high purity polysilicon by using the system. The system comprises a silicon material melting device arranged in a closed cavity, an electromigration device and an orientation solidification device, wherein the silicon material melting device and the electromigration device are connected through a first overflow pipe, and the electromigration device and the orientation solidification device are connected through a second overflow pipe. The method is characterized in that a horizontal direct current electric field which is vertical to the flowing direction of silicon liquid is forced on melted silicon liquid, cation impurities and anion impurities in the silicon liquid respectively migrate towards the direction of a cathode and the direction of an anode under the function of an electric field and gather in electrode regions at both sides, high impurity concentration silicon liquid and high purity silicon liquid are separated by a division baffle, the high purity silicon liquid is treated by orientation solidification ingot casting, and finally, a high purity polysilicon ingot is obtained. The invention can realize large scale continuous purifying production of high purity silicon and has the advantages of favorable purifying effect, simple equipment, little investment and low production cost.
Description
Technical field
The present invention relates to a kind of purification system that is used to prepare high purity polycrystalline silicon, reach method with this systems produce high purity polycrystalline silicon.
Background technology
Along with the fast development of photovoltaic industry, the polycrystalline silicon raw material demand of producing crystal-silicon solar cell is increasing.High purity polycrystalline silicon mainly is that though the polysilicon purity height that this method obtains, the production process energy consumption is excessive, and it is held at high price, and can not satisfy the low-cost demand for development of solar cell by the production of improvement Siemens Method at present, has hindered popularizing of photovoltaic generation.In recent years, new technology, the novel method of some preparation solar-grade polysilicons have obtained fast development, not only comprise traditional purifying techniques such as external refining, vacuum refinement, hydrometallurgy, directional freeze, comprise that also beam-plasma removes advanced smelting technologyes such as boron and electron beam dephosphorization.
Fused salt electrolysis is a key industry production method of producing light metal, also is unique method.As metals such as magnesium, aluminium, calcium, lithium, sodium all is to make with fused salt electrolysis process, and wherein the fused salt electrolysis of aluminium, magnesium has formed large-scale commercial production.People also obtain HIGH-PURITY SILICON to fused salt electrolysis process and have carried out useful trial, Chinese patent application numbers 200710065906.1 discloses a kind of preform (silicon-dioxide) reduction of fused salts of will giving up and has generated HIGH-PURITY SILICON, and the combined vacuum refining treatment prepares the method for solar energy level silicon then.A kind of preparation method of HIGH-PURITY SILICON is proposed in the Chinese patent application numbers 200910084349.7, with the mixed powder of industrial silicon and high purity copper is anode, with the rafifinal is that negative electrode carries out fused salt electrolysis, at first obtain aluminum silicon alloy, the array mode that adopts electromagnetic induction melting, fractional crystallization, vacuum distilling to purify then obtains HIGH-PURITY SILICON.More than two patents adopted different molten salt electrolysis methods, although the final silicon materials purity that obtains is higher, electrolytic process efficient is too low, and must cooperate complicated aftertreatment technology, therefore also is not suitable for large-scale production application.
Electromigration is purified and is applied to the purification production of rare earth metal usually, but because required current density is big, the time is long, still fails to be used for purifying metals in a large number, only produces ultra-high purity metal in a small amount at present in some research field.Introduced a kind of electromigration method of purification of silicon among the Japanese patent laid-open 6-206719, under the situation of not using fused salt, two electrodes are inserted in the molten silicon liquid, impurity in the silicon melt of energising back is subjected to electric field action, and anode and cathode zone are assembled respectively, behind the certain hour, two electrodes of quick cooling solidify near the silicon liquid of the enrichment impurity of electrode on electrode, take out electrode, thereby play impurity-eliminating effect.Though this kind method can reach the purpose of purification to a certain extent, complicated operation under the hot conditions can only carry out on small test device, is difficult in the actual production and uses, and more can't realize the successive suitability for industrialized production, and production efficiency is too low.
Summary of the invention
In order to solve the problem that above-mentioned prior art exists, the objective of the invention is to propose a kind of purification system of the high purity polycrystalline silicon of purifying, reach method with this systems produce high purity polycrystalline silicon.Adopt system of the present invention and preparation method can realize the large scale continuous prod of high purity polycrystalline silicon.
The purification system of high purity polycrystalline silicon of the present invention comprises: the silicon material melting appartus, electromigration device and the device for directionally solidifying that place airtight cavity.Silicon material melting appartus is connected by first upflow tube with the electromigration device, and the electromigration device is connected by second upflow tube with device for directionally solidifying.
Described silicon material melting appartus is made up of the fusion crucible that places the Medium frequency induction circle, and above fusion crucible, airtight cavity end face is mounted with vacuum feeding device.First upflow tube stretches in the fusion crucible from middle, fusion crucible bottom, stretch into and highly be 1/3 to 2/3 of the fusion crucible degree of depth, the upper port of first upflow tube is mounted with and prevents that silico briquette from falling into the material distributing cone of upflow tube, the electromigration incubation cavity is passed in the lower end of first upflow tube, and the silicon liquid of fusing flows into an end of electromigration groove by first upflow tube.
Described electromigration device comprises: make somebody a mere figurehead the electromigration groove in the electromigration incubation cavity, be respectively arranged with battery lead plate in the relative both sides of electromigration slot length direction, the direct supply external by lead and closed chamber is connected.The other end of electromigration groove has three horizontal uniform upflow tubes that penetrate from migration incubation cavity bottom in the electromigration groove, stretching into of these three upflow tubes highly is 1/3 to 2/3 of electromigration groove depth, separate by the distributing damper that is fixed on electromigration groove lateral sidewalls between them, wherein one of intermediary is second upflow tube of collecting HIGH-PURITY SILICON liquid, the 3rd upflow tube for collection high impurity concentration silicon liquid on both sides, the 3rd upflow tube leads to accumulator tank, second upflow tube leads in the solidification crucible of directional solidification furnace, the height of distributing damper is higher than the height that stretches into upflow tube in the electromigration groove, and the length of distributing damper is 2 to 3 times of overfall tube diameter.
Described device for directionally solidifying is equipped with solidification crucible by placing the lifting gantry that solidifies incubation cavity on the lifting gantry, be provided with resistance heater around the solidification crucible.Lifting gantry is by they sup-port, by the external lifting device control of closed chamber.
The method of purification step of high purity polycrystalline silicon of the present invention is as follows:
A. at first airtight cavity is vacuumized or feeds protective gas; add the silicon material by feeding device to the fusion crucible of silicon material smelting furnace; simultaneously the intermediate frequency induction heating circle is applied power; make the silicon material be fused into silicon liquid; and make silicon liquid reach the height of the upflow tube in the fusion crucible; keep the silicon liquid temp to be stabilized in 1450～1600 ℃, make silicon liquid have good flowability.
B. continue to add the silicon material subsequently, silicon liquid is flowed in the electromigration groove by first upflow tube, simultaneously the battery lead plate in the electromigration groove is applied electric field, along with silicon liquid in the electromigration groove increases, when liquid level reaches the height of the upflow tube in the electromigration groove in the electromigration groove, make the current density in the silicon liquid reach 1～100A/cm
2, the silicon liquid temp maintains 1450～1600 ℃.
C. along with flowing into from electromigration groove one end, silicon liquid flows out from the other end upflow tube, in the electromigration groove, can form directed flow at the uniform velocity, regulate the silicon material and add speed, the residence time of silicon liquid in the electromigration groove reached more than 10 minutes, under the effect of DC electric field, silicon liquid is after electromigration, through the distributing damper shunting, the higher silicon liquid of middle purity carries out ingot casting in the crucible of second upflow tube inflow directional solidification furnace, the silicon liquid that both sides purity is lower flows into accumulator tank through the 3rd upflow tube and treats to handle again.
D. before electromigration groove silicon liquid flows into the directional freeze crucible of device for directionally solidifying, the adjusting resistance heater is heated to 1420～1500 ℃ with the temperature of directional freeze crucible, along with the silicon liquid height in the directional freeze crucible increases, drive lifting device, the platform that descends gradually reduces the temperature of crucible bottom, and crystal begins upwards growth from crucible bottom, regulate heating power and dropping speed of the crucible, making the crystalline speed of growth is 5～50mm/h.
E. at last directional freeze is obtained high-purity polycrystal silicon ingot, cut head and afterbody, and the part that contacts with crucible all around, remaining part can be directly used in the microsection manufacture solar cell.
Advantage of the present invention is:
1) refining effect is good, and whole technology not only has electromigration purification effect, also has directional freeze purification effect.
2) equipment is simple, and employed equipment is common equipment in the whole process flow, realizes that easily scale of investment is little.
3) production efficiency height can be realized large scale continuous prod.No troublesome operation, the level of automation height.
4) pollution-free, whole flow process does not have generations such as waste gas, waste water, waste residue, and operating environment is good.
Description of drawings
Fig. 1 is the structural representation of purification system of the present invention;
Fig. 2 is the vertical view of the electromigration groove among Fig. 1;
Fig. 3 is the A-A diagrammatic cross-section of electromigration groove among Fig. 2.
Embodiment
Below in conjunction with accompanying drawing the specific embodiment of the present invention is described in further detail:
See Fig. 1, the purification system of high purity polycrystalline silicon of the present invention comprises: the silicon material melting appartus 2, electromigration device 3 and the device for directionally solidifying 4 that place airtight cavity 1.Silicon material melting appartus is connected by first upflow tube 21 with the electromigration device, and the electromigration device is connected by second upflow tube 31 with device for directionally solidifying.
Described silicon material melting appartus is made up of the fusion crucible 23 that places Medium frequency induction circle 22, and above fusion crucible, the end face of airtight cavity 1 is mounted with vacuum feeding device 5.First upflow tube 21 stretches in the fusion crucible from middle, fusion crucible bottom, stretch into and highly be 1/3 to 2/3 of the fusion crucible degree of depth, the upper port of first upflow tube is mounted with and prevents that silico briquette from falling into the material distributing cone 51 of upflow tube, electromigration incubation cavity 32 is stretched in the lower end of first upflow tube 21, and the silicon liquid of fusing flows into an end of electromigration groove 33 by first upflow tube.
Described electromigration device 3 comprises: make somebody a mere figurehead the electromigration groove 33 in electromigration incubation cavity 32, be respectively arranged with battery lead plate 34 in the relative both sides of the length direction of electromigration groove, be connected by lead and airtight cavity 1 outer direct supply (not drawing among Fig. 1).The other end of electromigration groove 33 has three horizontal uniform upflow tubes that penetrate from electromigration incubation cavity 32 bottoms in the electromigration groove, stretching into of these three upflow tubes highly is 1/3 to 2/3 of electromigration groove depth, separate by the distributing damper 35 that is fixed on electromigration groove lateral sidewalls between them, wherein one of intermediary is second upflow tube 31 of collecting HIGH-PURITY SILICON liquid, both sides are for collecting the 3rd upflow tube 36 of high impurity concentration silicon liquid, the 3rd upflow tube leads to accumulator tank 37, second upflow tube leads to solidification crucible 41 tops of device for directionally solidifying 4, the height of distributing damper 35 will be higher than upflow tube height in the electromigration groove, and the length of distributing damper is 2 to 3 times of overfall tube diameter.Battery lead plate 34 adopts high purity graphite to make, and battery lead plate is parallel with silicon liquid flow direction.
Electromigration device role of the present invention is: apply one and the vertical horizontal DC electric field of flow direction on the molten silicon liquid of sluggish flow.At silicon liquid mobile simultaneously, impurity electrode region to both sides under effect of electric field moves, be that positively charged ion or the impurity with cationic characteristic (below be referred to as cation impurity) move to cathode direction, negatively charged ion or have impurity (below be referred to as anionic impurity) the anode direction migration of anion characteristic, thus both sides concentration height, Impurity Distribution state that intermediate concentration is low on the cross section that vertical silicon liquid flows to, formed.Adopt the distributing damper silicon liquid that purified silicon liquid in centre and both sides foreign matter content is high to separate, make them flow into different containers respectively, reach the purpose of purified silicon.
Described device for directionally solidifying 4 comprises: place the solidification crucible 41 that is equipped with resistance heater 44 on every side that solidifies incubation cavity 42, solidification crucible 41 places on the lifting gantry 43, lifting gantry is supported by support bar 45, by external apparatus for controlling of lifting 46 controls of closed chamber.
Method of purification of the present invention mainly comprises three aspects:
1) control silicon flow velocity: the silicon material that will need to purify places the fusing of silicon material melting appartus internal heating, and the mode that adopts Frequency Induction Heating is with the silico briquette fast thawingization, and the silicon liquid temp is stabilized in 1450～1600 ℃, makes it keep good flowability.Add the silicon material gradually, make silicon liquid flow into electromigration groove one end, in the electromigration groove, form the directed flow of silicon liquid by upflow tube.Control the flow velocity of silicon liquid by regulating feed rate at the electromigration groove, silicon liquid flows into from electromigration groove one end, and from the upflow tube outflow of the other end, the residence time can not be less than 10 minutes, for 1 meter long electromigration groove, the velocity of flow of silicon liquid should be less than 0.1 meter/minute.
2) control strength of electric field: be parallel to silicon liquid flow direction in electromigration groove both sides electrode is set, connect direct supply, make the horizontal component of electric field that forms vertical silicon liquid flow direction in the silicon liquid.The size of strength of electric field is decided according to actual conditionses such as electromigration groove shape, heat-insulating properties, and general current density is controlled at 1～100A/cm
2Between, the joule heating that the assurance electric current produces in silicon liquid is enough kept the silicon liquid temp, and makes it have good flowability.
3) shunting: cation impurity and anionic impurity under the highfield effect respectively to the negative electrode of electromigration groove both sides and anode direction migration, near and enrichment electrode.When silicon liquid when after a while electromigration flows near overflow port, adopt distributing damper that the high impurity concentration silicon liquid of intermediary HIGH-PURITY SILICON liquid with both sides is separated, make in the crucible of HIGH-PURITY SILICON liquid by upflow tube inflow device for directionally solidifying and carry out ingot casting, high impurity concentration silicon liquid flows into returnable, processing to be recycled.
Claims (2)
1. the purification system of a high purity polycrystalline silicon comprises: place silicon material melting appartus (2), electromigration device (3) and the device for directionally solidifying (4) of airtight cavity (1), it is characterized in that:
Silicon material melting appartus is connected by first upflow tube (21) with the electromigration device, and the electromigration device is connected by second upflow tube (31) with device for directionally solidifying;
Described silicon material melting appartus (2) is made up of the fusion crucible that places Medium frequency induction circle (22) (23), and above fusion crucible, the end face of airtight cavity (1) is mounted with vacuum feeding device (5); First upflow tube (21) stretches in the fusion crucible (23) from middle, fusion crucible bottom, stretch into and highly be 1/3 to 2/3 of the fusion crucible degree of depth, the upper port of first upflow tube is mounted with and prevents that silico briquette from falling into the material distributing cone of upflow tube (51), electromigration incubation cavity (32) is stretched in the lower end of first upflow tube (21), and the silicon liquid of fusing flows into an end of electromigration groove (33) by first upflow tube;
Described electromigration device (3) comprising: make somebody a mere figurehead the electromigration groove (33) in electromigration incubation cavity (32), be respectively arranged with battery lead plate (34) in the relative both sides of the length direction of electromigration groove, the direct supply outer by lead and airtight cavity (1) is connected; The other end of electromigration groove (33) has three horizontal uniform upflow tubes that penetrate from electromigration incubation cavity (32) bottom in the electromigration groove (33), stretching into of these three upflow tubes highly is 1/3 to 2/3 of electromigration groove depth, separate by the distributing damper that is fixed on electromigration groove lateral sidewalls (35) between them, wherein one of intermediary is second upflow tube (31) of collecting HIGH-PURITY SILICON liquid, both sides are for collecting the 3rd upflow tube (36) of high impurity concentration silicon liquid, the 3rd upflow tube leads to accumulator tank (37), second upflow tube leads in the solidification crucible (41) of device for directionally solidifying (4), the height of distributing damper (35) is higher than the height of second upflow tube, and the length of distributing damper is 2 to 3 times of overfall tube diameter;
Described device for directionally solidifying (4) comprising: place the solidification crucible (41) that is equipped with resistance heater (44) on every side that solidifies incubation cavity (42), solidification crucible (41) places on the lifting gantry (43), lifting gantry is supported by support bar (45), is controlled by the external apparatus for controlling of lifting of closed chamber (46).
2. the method for purification of a high purity polycrystalline silicon is characterized in that step is as follows:
A. at first airtight cavity (1) is vacuumized or feeds protective gas, add the silicon material by feeding device (5) to the fusion crucible (23) of silicon material melting appartus (2), simultaneously intermediate frequency induction heating circle (22) is applied power, make the silicon material be fused into silicon liquid, and make silicon liquid reach the height of first upflow tube (21) in the fusion crucible, keep the silicon liquid temp to be stabilized in 1450～1600 ℃, make silicon liquid have good flowability;
B. continue to add the silicon material subsequently, silicon liquid is flowed in the electromigration groove (33) by first upflow tube (21), simultaneously the battery lead plate in the electromigration groove (34) is applied electric field, along with silicon liquid in the electromigration groove increases, when liquid level reaches the height of the upflow tube in the electromigration groove in the electromigration groove, make the current density in the silicon liquid reach 1～100A/cm
2, keep the silicon liquid temp at 1450～1600 ℃;
C. silicon liquid flows into from electromigration groove one end and flows out from the other end overflow, in the electromigration groove, form directed flow at the uniform velocity, regulate the silicon material and add speed, the residence time of silicon liquid in the electromigration groove reached more than 10 minutes, under the effect of DC electric field, silicon liquid is after electromigration, through the distributing damper shunting, the higher silicon liquid of middle purity flows in the solidification crucible (41) through second upflow tube (31) and carries out ingot casting, and the silicon liquid that both sides purity is lower flows into accumulator tank (37) through the 3rd upflow tube (36) and treats to handle again;
D. the directional freeze crucible (41) that flows into device for directionally solidifying (4) at electromigration groove silicon liquid before, regulate resistance heater (44), temperature is heated to 1420～1500 ℃, along with the silicon liquid height in the directional freeze crucible increases, drive lifting device (46), platform (43) is descended gradually, the temperature of crucible bottom is reduced, crystal begins upwards growth from crucible bottom, regulates heating power and dropping speed of the crucible, and making the crystalline speed of growth is 5～50mm/h;
E. at last directional freeze is obtained high-purity polycrystal silicon ingot, cut head and afterbody, and the part that contacts with crucible all around, remaining part can be directly used in the microsection manufacture solar cell.
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| CN103072994A (en) * | 2013-02-04 | 2013-05-01 | 福建兴朝阳硅材料股份有限公司 | Electrophoretic assistant slag forming and boron removing method |
| CN109112618A (en) * | 2017-06-23 | 2019-01-01 | 镇江仁德新能源科技有限公司 | A kind of directional solidification growth device and method of solar energy polycrystalline silicon |
| CN113108595A (en) * | 2021-02-23 | 2021-07-13 | 昆明理工大学 | Industrial molten pool visualization system and method based on electromagnetic tomography technology |
| US11242615B2 (en) * | 2018-12-14 | 2022-02-08 | The 13Th Research Institute Of China Electronics Technology Group Corporation | Growth method and apparatus for preparing high-yield crystals |
| CN115323491A (en) * | 2022-07-28 | 2022-11-11 | 商南中剑实业有限责任公司 | Device and method for preparing high-purity silicon through directional solidification of silicon and copper |
| CN115537587A (en) * | 2022-05-27 | 2022-12-30 | 鲍少聪 | Equipment for purifying coarse rare earth metal under solid phase |
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| CN103072994A (en) * | 2013-02-04 | 2013-05-01 | 福建兴朝阳硅材料股份有限公司 | Electrophoretic assistant slag forming and boron removing method |
| CN109112618A (en) * | 2017-06-23 | 2019-01-01 | 镇江仁德新能源科技有限公司 | A kind of directional solidification growth device and method of solar energy polycrystalline silicon |
| US11242615B2 (en) * | 2018-12-14 | 2022-02-08 | The 13Th Research Institute Of China Electronics Technology Group Corporation | Growth method and apparatus for preparing high-yield crystals |
| CN113108595A (en) * | 2021-02-23 | 2021-07-13 | 昆明理工大学 | Industrial molten pool visualization system and method based on electromagnetic tomography technology |
| CN115537587A (en) * | 2022-05-27 | 2022-12-30 | 鲍少聪 | Equipment for purifying coarse rare earth metal under solid phase |
| CN115323491A (en) * | 2022-07-28 | 2022-11-11 | 商南中剑实业有限责任公司 | Device and method for preparing high-purity silicon through directional solidification of silicon and copper |
| CN115323491B (en) * | 2022-07-28 | 2023-09-19 | 商南中剑实业有限责任公司 | Device and method for preparing high-purity silicon through directional solidification of silicon copper |
| CN117548037A (en) * | 2024-01-11 | 2024-02-13 | 长盛(廊坊)科技有限公司 | PAN-based carbon fiber auxiliary agent delivery device and delivery method thereof |
| CN117548037B (en) * | 2024-01-11 | 2024-03-29 | 长盛(廊坊)科技有限公司 | PAN-based carbon fiber auxiliary agent delivery device and delivery method thereof |
| CN117685576A (en) * | 2024-02-02 | 2024-03-12 | 济南格欧环保科技有限公司 | Transfer arc plasma melting fly ash equipment with mechanical motion electrode |
| CN117685576B (en) * | 2024-02-02 | 2024-04-16 | 济南格欧环保科技有限公司 | Transfer arc plasma melting fly ash equipment with mechanical motion electrode |
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