CN103351002B - Polysilicon directional solidification device - Google Patents
Polysilicon directional solidification device Download PDFInfo
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- CN103351002B CN103351002B CN201310307458.7A CN201310307458A CN103351002B CN 103351002 B CN103351002 B CN 103351002B CN 201310307458 A CN201310307458 A CN 201310307458A CN 103351002 B CN103351002 B CN 103351002B
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- quartz crucible
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Abstract
The invention relates to the field of polysilicon purification, in particular to a polysilicon directional solidification device which comprises a furnace body, a quartz crucible is placed in the furnace, a graphite heating unit, an insulating sleeve and a induction coil are arranged on the outer wall of the quartz crucible from inside to outside in sequence in a surrounding manner, an ingot mechanism communicated with the bottom of the furnace body is arranged at the bottom of the quartz crucible, the height of the insulating sleeve is 1.5 to 2 time higher of that of the quartz crucible, a graphite spiral plate is arranged at the upper part of the ingot mechanism, a spiral channel built in the graphite spiral plate is communicated with the inlet of the ingot mechanism, and outlets are formed in the edge of the two sides of the graphite spiral plate. According to the device, thermal radiation of the sidewall of the quartz crucible generated in the pulling process can be better intercepted, thermal radiation of the sidewall of the quartz crucible is effectively decreased, and the directional solidification effect is better than conventional solidification method. The device is short in warming up time, small in insulating energy consumption, controllable in cooling speed, the crystal growth is better in cooling method when compared with conventional mode, and can better realize directional solidification effect.
Description
Technical field
The invention belongs to field of polycrystalline silicon purification, be specifically related to a kind of Polysilicon directional solidification device.
Background technology
At present, China has become world energy sources production and consumption big country, but per capita energy's level of consumption is also very low.Along with development that is economic and society, China's energy demand is by sustainable growth, for current energy shortage situation, deep thinking is all being carried out in countries in the world, and make great efforts to improve efficiency of energy utilization, promote the development and application of renewable energy source, reduce the dependence to Imported oil, strengthen energy security.
Solar energy power generating development in recent years as one of the important development direction of renewable energy source is swift and violent, and its proportion is increasing.According to " planning of renewable energy source Long-and Medium-term Development ", to the year two thousand twenty, China strives making solar electrical energy generation installed capacity reach 1.8GW(gigawatt), will 600GW be reached to the year two thousand fifty.Expect the year two thousand fifty, the electric power installation of Chinese renewable energy source will account for 25% of national electric power installation, and wherein photovoltaic generation installation will account for 5%.Before estimating the year two thousand thirty, the compound growth rate of Chinese sun power installed capacity will up to more than 25%.
The development of solar photovoltaic industry depends on the purification to polycrystalline silicon raw material.In the process of purifying to polycrystalline silicon raw material, there is crucial, a requisite link, carry out directional freeze purification to polycrystalline silicon raw material exactly, used directional solidification technique is widely used in field of metallurgy purification.The segregation coefficient in polycrystalline silicon raw material between silicon and metallic impurity is utilized to there is this feature of larger difference, in process of setting, first the silicon liquid of quartz crucible bottom start to solidify, for reaching fractional condensation balance, the impurity that segregation coefficient is little is out gathered in liquid state to the continuous separation by diffusion of liquid state from the silicon solidified, constantly carry out along with solidifying, the concentration of metallic impurity in liquid state is more and more higher, finally solidify on the top of ingot casting, for some time is incubated at relatively high temperatures after having solidified, each composition is made fully to spread to reach fractional condensation balance, finally one end higher for metals content impurity is removed, obtain the polycrystalline silicon ingot casting of purifying.
Current directional solidification technique all adopts the drop-down mode of quartz crucible to make polysilicon directional freezing substantially, drop-down is that quartz crucible is pulled out thermal field region gradually, because the height and quartz crucible that are incubated sleeve are at present basically identical, so drop-down quartz crucible part is exposed in body of heater, a large amount of heats can be distributed as surrounding, the quartz crucible outside wall temperature of drop-down part is caused to be less than core temperature, polysilicon can be there is along sidewall towards central growth in which, cause metallicity impurity in polysilicon to from four circumferential center enrichments, light then affect directional freeze impurity-eliminating effect, heavy then cause qualitative solidify purifying polycrystalline silicon failure.In addition, directional solidification technique all adopts ingot pulling mechanism top to adopt the design of water-cooled copper dish to carry out circulating water to bottom quartz crucible substantially, silicon melt is made to carry out directional freeze, the low-temperature receiver of this kind of mode all exists in the whole process of melting, a large amount of heat energy can be taken away by this mode, thus increases energy consumption.
Summary of the invention
According to above the deficiencies in the prior art, the present invention proposes a kind of Polysilicon directional solidification device, make polysilicon be in keeping warm mode in directional freeze process always, polysilicon oriented growth completely from bottom to top in solidifying can be realized, improve the impurity-eliminating effect of polysilicon in directional freeze, adopt using argon gas as the low-temperature receiver in process of setting, can realize only in process of setting, adding low-temperature receiver, fusing and holding stage, without low-temperature receiver, significantly improve the utilization ratio of energy, reduce the consumption of energy.
A kind of Polysilicon directional solidification device of the present invention, comprise body of heater, quartz crucible is placed with in body of heater, quartz crucible outer wall is surrounded with graphite heater, insulation sleeve and ruhmkorff coil from inside to outside successively, the ingot pulling mechanism led to bottom of furnace body is provided with bottom quartz crucible, the height of insulation sleeve is 1.5 ~ 2 times of quartz crucible height, the top of ingot pulling mechanism is graphite spiral plate, the built-in helical channel of graphite spiral plate is connected with the inlet mouth of ingot pulling mechanism, the air outlet that the both sides of the edge place of graphite spiral plate has.
Preferably be provided with graphite supporting plate between quartz crucible and ingot pulling mechanism, and graphite supporting plate is fitted with insulation sleeve lining.Owing to being subject to recycle gas cooling bottom quartz crucible, so larger thermal shocking can be subject to, easily damaging quartz crucible, therefore between quartz crucible and ingot pulling mechanism, be provided with graphite supporting plate, prevent thermal shocking from causing the explosion of quartz crucible.
The height of insulation sleeve is preferably 2 times of quartz crucible height.When the height being incubated sleeve is quartz crucible height 2 times time, can ensure that polysilicon is in the enclosing region of insulation sleeve in directional freeze process always.
In helical channel body of ventilating be preferably argon gas.The gas being generally used for cooling is rare gas element, and in rare gas element, the cost of argon gas is minimum, and therefore the present invention preferably uses argon gas as cooling gas.Argon gas in helical channel is selected under normal temperature, and namely inlet air temperature is preferably at 5 ~ 30 DEG C.
Helical channel is preferably double-spiral structure.Double-spiral structure design ensure that gas fully flows in helical channel, increases heat exchanger effectiveness.
In the present invention, graphite spiral plate is for being divided into upper and lower two portions: top is divided into the graphite cake with flight, and bottom is divided into graphite cake, and upper and lower two portions form a breather with helical channel jointly.Gas is discharged by air outlet, outside insulation sleeve, discharges body of heater from the upper bell opening part of body of heater.
Working process of the present invention is as follows:
(1) be positioned in quartz crucible by silicon material, unlatching mechanical pump, lobe pump vacuumize body of heater.
(2) open ruhmkorff coil, to graphite heater effect, silicon material in quartz crucible is heated up and melts formation silicon melt.
(3), after insulation, lobe pump and mechanical pump is closed successively.In body of heater, be filled with argon gas, start ingot pulling mechanism;
(4) quartz crucible drop-down before, first thermopair is positioned at the unsettled placement of quartz crucible outer bottom, the melt of Real-Time Monitoring silicon and solid interface temperature, when the temperature shown is higher than 1414 DEG C, continue to increase gas ventilation amount, when temperature is lower than 1414 DEG C, reduces gas ventilation amount, make the speed of cooling of silicon melt consistent with the lowering speed of ingot pulling mechanism.
(5) until silicon melt is completely cooled solidify after, stop ruhmkorff coil energising, stop ingot pulling mechanism motor rotation, operation terminates.
The invention has the advantages that: this device can realize the oriented growth of silicon melt, can be good at realizing the object that directional freeze removes metallicity impurity in polysilicon.This device is used to can be good at, by the thermal radiation interception of Quartz crucible lateral wall in downdraw process, effectively reducing the heat loss through radiation of sidewall, making directional solidification effect more conventional directional freeze mode better.The crystal grain that sidewall grows to center position reduces more than 90% relative to conventional equipment.The heating-up time of this device is short, and during insulation, energy consumption is little, and simultaneously speed of cooling can control, and the more conventional type of cooling of crystal growth is good, can better realize the effect of directional freeze.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention;
Fig. 2 is the A-A view of in Fig. 17;
Fig. 3 is the structural representation of prior art;
In figure: 1, body of heater 2, quartz crucible 3, graphite heater 4, insulation sleeve 5, ruhmkorff coil 6, ingot pulling mechanism 7, graphite spiral plate 8, inlet mouth 9, air outlet 10, graphite supporting plate 11, water-cooled ingot pulling mechanism.
Embodiment
Below in conjunction with drawings and Examples, the present invention will be further described.
Embodiment 1:
As shown in FIG. 1 to 3, a kind of Polysilicon directional solidification device, comprise body of heater 1, quartz crucible 2 is placed with in body of heater 1, quartz crucible 2 outer wall is surrounded with graphite heater 3 from inside to outside successively, insulation sleeve 4 and ruhmkorff coil 5, be provided with bottom quartz crucible 2 with body of heater 1 bottom the ingot pulling mechanism 6 that leads to, the height of insulation sleeve 4 is 2 times of quartz crucible 2 height, the top of ingot pulling mechanism 6 is graphite spiral plate 7, the built-in helical channel of graphite spiral plate 7 is connected with the inlet mouth 8 of ingot pulling mechanism 6, the air outlet 9 that the both sides of the edge place of graphite spiral plate 7 has.
Be provided with graphite supporting plate 10 between quartz crucible 2 and ingot pulling mechanism 6, and graphite supporting plate 10 is fitted with insulation sleeve 4 inwall.Owing to being subject to recycle gas cooling bottom quartz crucible 2, so larger thermal shocking can be subject to, easily damages quartz crucible 2, therefore between quartz crucible 2 and ingot pulling mechanism 6, be provided with graphite supporting plate 10, prevent thermal shocking from causing the explosion of quartz crucible 2.
When the height being incubated sleeve 4 is quartz crucible height 2 times time, can ensure that polysilicon is in the enclosing region of insulation sleeve 4 in directional freeze process always.
In helical channel body of ventilating be argon gas.The gas being generally used for cooling is rare gas element, and in rare gas element, the cost of argon gas is minimum, and therefore this device preferably uses argon gas as cooling gas.Argon gas in helical channel is selected under normal temperature, and namely inlet air temperature is at 5 ~ 30 DEG C.
Helical channel is double-spiral structure.Double-spiral structure design ensure that gas fully flows in helical channel, increases heat exchanger effectiveness.
In this device, graphite spiral plate 7 is for being divided into upper and lower two portions: top is divided into the graphite cake with flight, and bottom is divided into graphite cake, and upper and lower two portions form a breather with helical channel jointly.Gas is discharged by air outlet 9, outside insulation sleeve 4, discharges body of heater from the upper bell opening part of body of heater 1.
Compared with prior art, difference is 2 points to this device: one is the lengthening being incubated sleeve 4; Two is change present recycle gas into by original circulating water to cool, and corresponding parts change to the ingot pulling mechanism 6. with graphite spiral plate 7 by water-cooled ingot pulling mechanism 11
Working process is as follows:
(1) industrial silicon 500kg is positioned in quartz crucible 2, opens mechanical pump and 800Pa is evacuated to body of heater 1, then open lobe pump and continue to be evacuated to 0.1Pa;
(2) open ruhmkorff coil 5, graphite heater 3 is acted on, makes silicon material in quartz crucible 2 be warming up to 1500 DEG C, after 10 hours, silicon material is heated up and melts formation silicon melt;
(3), after being incubated 8 hours, lobe pump and mechanical pump is closed successively.In body of heater 1, be filled with argon gas, start ingot pulling mechanism 6;
(4) quartz crucible 2 drop-down before, first thermopair is positioned at the unsettled placement of quartz crucible 2 outer bottom, the melt of Real-Time Monitoring silicon and solid interface temperature, when the temperature shown is higher than 1414 DEG C, continue to increase gas ventilation amount, when temperature is lower than 1414 DEG C, reduces gas ventilation amount, make the speed of cooling of silicon melt consistent with the lowering speed of ingot pulling mechanism 6.
(5) until silicon melt is completely cooled solidify after, stop being energized to ruhmkorff coil 5, stop ingot pulling mechanism motor rotation, operation terminates.
For the silicon material of 500kg, under identical intensification power 200KW, the prior art heating-up time is 11.75h, and this device heat-up rate comparatively conventional equipment is fast, is only 10.5h; Holding stage, prior art needs 76kW, and after adopting this device, holding stage power only needs 58kW.Solidification stages conventional chilling mode can only cool with same speed of cooling, uses this device to realize speed of cooling controlled, and namely argon flow amount can conveniently regulate, and crystal growth comparatively conventional chilling mode is good, realize the effect of directional freeze preferably.
Claims (3)
1. a Polysilicon directional solidification device, comprise body of heater, quartz crucible is placed with in body of heater, quartz crucible outer wall is surrounded with graphite heater, insulation sleeve and ruhmkorff coil from inside to outside successively, the ingot pulling mechanism led to bottom of furnace body is provided with bottom quartz crucible, the height that it is characterized in that being incubated sleeve is 1.5 ~ 2 times of quartz crucible height, the top of ingot pulling mechanism is graphite spiral plate, the built-in helical channel of graphite spiral plate is connected with the inlet mouth of ingot pulling mechanism, and the both sides of the edge place of graphite spiral plate has air outlet.
2. Polysilicon directional solidification device according to claim 1, is characterized in that being provided with graphite supporting plate between quartz crucible and ingot pulling mechanism, and graphite supporting plate is fitted with insulation sleeve lining.
3. Polysilicon directional solidification device according to claim 1, the height that it is characterized in that being incubated sleeve is 2 times of quartz crucible height.
4.polysilicon directional solidification device according to claim 1, to it is characterized in that in helical channel body of ventilating be argon gas.
5.polysilicon directional solidification device according to claim 4, is characterized in that the inlet air temperature of the argon gas in helical channel is 5 ~ 30 DEG C.
6.polysilicon directional solidification device according to claim 1, is characterized in that helical channel is double-spiral structure.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201310307458.7A CN103351002B (en) | 2013-07-20 | 2013-07-20 | Polysilicon directional solidification device |
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| CN201310307458.7A CN103351002B (en) | 2013-07-20 | 2013-07-20 | Polysilicon directional solidification device |
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| CN103351002B true CN103351002B (en) | 2015-01-07 |
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| CN106946260A (en) * | 2017-04-13 | 2017-07-14 | 苏州振吴电炉有限公司 | HIGH-PURITY SILICON purification production fractional condensation device |
| CN107790689B (en) * | 2017-10-30 | 2020-01-14 | 中国航发动力股份有限公司 | Water-cooling copper disc device for improving circulating water cooling effect and machining method thereof |
| CN110655075B (en) * | 2019-10-25 | 2024-05-28 | 清华大学深圳国际研究生院 | Continuous high-temperature purification equipment |
| CN111649579A (en) * | 2020-04-27 | 2020-09-11 | 江苏搏斯威化工设备工程有限公司 | Heat conduction rake of vacuum rake dryer |
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| CN101289188B (en) * | 2008-05-30 | 2010-06-02 | 大连理工大学 | Process and device for removing phosphorus and metal impurities in polycrystalline silicon |
| CN102976333B (en) * | 2012-12-13 | 2014-07-09 | 青岛隆盛晶硅科技有限公司 | Method and equipment for controlled directional solidification and purification of polycrystalline silicon through taking tailing by graphite tube |
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Effective date of registration: 20171108 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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Effective date of registration: 20171215 Address after: Shandong province Qingdao Jimo 266234 Pu Dong Zhen Ren Jia Tun Cun Ren Jia Tun Lu City Patentee after: QINGDAO NEW ENERGY SOLUTIONS INC. (NESI) 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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