CN102849743B - Polysilicon purification method and device by reverse induced solidification - Google Patents
Polysilicon purification method and device by reverse induced solidification Download PDFInfo
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Abstract
The invention relates to a polysilicon purification method and a polysilicon purification device by reverse induced solidification, falling into the technical field of metallurgy purification. The method comprises the steps of heating and melting silicon material into molten silicon through an induction coil; reducing power of the induction coil; downwardly pulling ingot through a water-cooled rotation rod to solidify molten silicon from bottom to top; starting a powder spreading device when solidification reaches 80-90%, to spread high-purity silicon powder in the upper layer molten silicon, and realize rapid reverse solidification of the upper layer molten silicon by using the high-purity silicon powder as nucleating agent; cutting off the upper layer reverse-solidified part after complete solidification, and collecting the lower layer casting ingot as high-purity silicon casting ingot. At solidification final stage, by the above rapid reverse solidification of upper layer molten silicon having high impurity content, diffusion of high-content impurities from the upper layer molten silicon toward the solidified low-concentration region during temperature holding process is effectively suppressed, to realize the objective of polysilicon purification by reverse induced solidification.
Description
Technical field
The invention belongs to metallurgy purification technical field, particularly the method for purification is solidified in a kind of reverse induction, also relates in addition its equipment.
Background technology
At present, China has become world energy sources production and consumption big country, but energy expenditure level is also very low per capita.Along with economical and social development, 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 effort improves 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 important development direction of renewable energy source is swift and violent, and its proportion is increasing.According to the preliminary statistics, China 2010 newly-increased grid-connected photovoltaic power generation installation 530,000 kW, accumulative total installation reaches 830,000 kW, ground large grid-connected photovoltaic power generation accumulative total 700,000 kW that install wherein, architecture-integral grid-connected photovoltaic power generation approximately 130,000 kW that install.The newly-increased installation in 2010 of photovoltaic generation market, the whole world is estimated to increase and surpass 120% on year-on-year basis, more than reaching 1,700 ten thousand kW, drives China's photovoltaic industry size to expand rapidly.
The development of photovoltaic industry depends on the purification to silicon raw material.In the process that silicon raw material is purified, there is crucial, a requisite link, exactly silicon raw material is carried out to directional freeze purification, directional solidification technique used is widely used in field of metallurgy purification.Utilize the segregation coefficient between silicon and impurity in silicon raw material to have this feature of larger difference, in process of setting, first the silicon liquid of 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 solidifying, along with solidifying constantly, carry out, the concentration of impurity in liquid state is more and more higher, under finally solidifying on the top of ingot casting, after having solidified, under comparatively high temps, be incubated for some time, make each composition fully spread to reach fractional condensation balance, finally the higher one end of foreign matter content is removed, obtain the polycrystalline silicon ingot casting of purifying.
Yet ingot casting is in the process of insulation, the impurity that those content are high can be to the low position diffusion of foreign matter content, make silicon purity along with the prolongation of soaking time reduces on the contrary gradually, this has affected refining effect, and in this case, the afterbody waste material of excision is up to 25% ~ 35%, and yield rate is only 65-75%, cause the significant wastage of the energy and raw material, also therefore increased manufacturing cost.
Summary of the invention
The present invention seeks to as overcoming above deficiency, provide a kind of reverse induction to solidify the method for purifying polycrystalline silicon, the method is used silica flour as nucleating agent, impurity is fixed on to the tail end of ingot casting, the counter diffusion of inhibition of impurities, improved purity, and the tailing of required excision can be reduced to 5% ~ 20%, energy and production cost have greatly been saved, another object of the present invention is to provide the equipment that purifying polycrystalline silicon is solidified in a kind of reverse induction, this device structure is simple, and easy handling is effectively realized the object that purification is solidified in oppositely induction.
The technical scheme that adopted is for achieving the above object: the method for purifying polycrystalline silicon is solidified in a kind of reverse induction, first adopt ruhmkorff coil that the silicon material in quartz crucible is heated to 1450 ~ 1550 ℃ and make it fusing formation silicon melt, starting afterwards water-cooled revolving bar moves downward and draws ingot, silicon melt is solidified to top by quartz crucible bottom, when solidifying while reaching 80% ~ 90%, by water-cooled revolving bar rotation quartz crucible, open powder discharging device is scattering in the upper strata silicon melt that foreign matter content is higher high-purity silicon powder simultaneously, high-purity silicon powder makes the rapid reverse solidification of upper strata silicon melt as nucleating agent, after having solidified, cut the part that upper strata reverse solidification obtains, the lower floor's ingot casting obtaining is HIGH-PURITY SILICON ingot casting.
The method of purifying polycrystalline silicon is solidified in described a kind of reverse induction, and the concrete steps that adopt are:
The first step pre-treatment: be 99.9% ~ 99.95% silicon raw material to the purity of adding quartz crucible volume 90% ~ 100% in quartz crucible, to packing high-purity silicon powder in powder discharging device, build bell, keep the stopping property in body of heater, with mechanical pump and lobe pump, will in body of heater, be evacuated to 1 ~ 10Pa respectively;
Second step melt, draw ingot: opening power, start ruhmkorff coil, silicon material is heated to 1450 ~ 1550 ℃, silicon material is melted completely, and be incubated 50 ~ 80min at 1450 ~ 1550 ℃, control the temperature difference in melt simultaneously, open afterwards water-cooled revolving bar, make it to move downward with the speed of 0.1-1mm/min, drive is solidified attemperator and is declined and draw ingot with same speed, makes silicon melt to top, carry out directional freeze by quartz crucible bottom;
The 3rd step reverse solidification is purified: when silicon melt solidifies while reaching 80% ~ 90%, by water-cooled revolving bar rotation quartz crucible, open powder discharging device simultaneously, high-purity silicon powder is dropped in melt, high-purity silicon powder is evenly distributed on bath surface along with the rotation of quartz crucible, further reduction along with temperature, the high-purity silicon powder adding is as nucleating agent, make the rapid reverse solidification of silicon melt that foreign matter content is higher, after having solidified, cut the part that upper strata reverse solidification obtains, the lower floor's ingot casting obtaining is HIGH-PURITY SILICON ingot casting, its purity will reach 99.99%-99.999%, yield rate reaches 80-95%.
The purity of described high-purity silicon powder is 99.999% ~ 99.9999%.
The equipment that a kind of method that purifying polycrystalline silicon is solidified in reverse induction adopts, by bell, body of heater and supporting base form external structure, it is characterized in that: water-cooled revolving bar is fixedly connected with water-cooled pallet through bottom of furnace body, heating panel is fixedly installed on water-cooled pallet, solidifying attemperator is positioned on heating panel, muff jacket casing is in solidifying attemperator periphery, insulation sleeve is fixedly installed in inboard wall of furnace body by fixed support, ruhmkorff coil is placed on outside insulation sleeve, powder discharging device is fixed on body of heater inside by bracing frame, and be positioned at and solidify directly over attemperator, mechanical pump and lobe pump are positioned over outside body of heater, by vacuum pipe, connect, body of heater inside is led in vacuum pipe one end.
Described water-cooled revolving bar is cylindric, built-in cooling water pipeline.
Described water-cooled pallet is discoid, built-in cooling water pipeline.
Described heating panel is discoid copper heating panel.
The described attemperator that solidifies is at least comprised of quartz crucible and plumbago crucible, adopts plumbago crucible to be positioned on heating panel, within quartz crucible is embedded in plumbago crucible.
Described insulation sleeve is the cylindric carbon fibre material insulation sleeve of two ends uncovered.
Unusual effect of the present invention is: solidifying the coda stage, utilize doffer that silica flour is evenly scattering into silicon melt surface, silica flour solidifies rapidly as nucleating agent the upper strata silicon melt that foreign matter content is higher, effectively suppressed the impurity that in the silicon melt of upper strata, content is higher spreads to the low concentration region having solidified in insulating process, reach reverse induction and solidified the object of purifying polycrystalline silicon, it is good that this equipment has refining effect, simple to operate, the advantage that controllability is strong.
Accompanying drawing explanation
Fig. 1. the device structure schematic diagram of purifying polycrystalline silicon is solidified in a kind of reverse induction
In figure, 1, bell, 2, powder discharging device, 3, bracing frame, 4, body of heater, 5, quartz crucible, 6, plumbago crucible, 7, insulation sleeve, 8, ruhmkorff coil, 9, fixed support, 10, heating panel, 11, supporting base, 12, water-cooled pallet, 13, water-cooled revolving bar, 14, mechanical pump, 15, lobe pump, 16, vacuum pipe.
Embodiment
Below in conjunction with specific embodiments and the drawings, describe the present invention in detail, but the present invention is not limited to specific embodiment.
The equipment of purifying polycrystalline silicon is solidified in a kind of reverse induction as shown in Figure 1, by bell 1, body of heater 4 and supporting base 11 form external structure, water-cooled revolving bar 13 is fixedly connected with water-cooled pallet 12 through body of heater 4 bottoms, the object of water-cooled revolving bar 13 is in purification process, to play to drive crucible to rotate, powder falling is evenly trickled down at bath surface, make crucible move downward with given pace simultaneously, draw ingot, the effect that water-cooled pallet 12 plays heat radiation and supports, heating panel 10 is fixedly installed in water-cooled pallet 12 tops, its main purpose is to accelerate the heat radiation of crucible bottom, make crucible top to forming a thermograde between bottom, be convenient to solidifying of crucible bottom melt, form ingot casting, solidifying attemperator is positioned on heating panel 10, solidifying attemperator is at least comprised of quartz crucible 5 and plumbago crucible 6, adopt plumbago crucible 6 to be positioned on heating panel 10, within quartz crucible 5 is embedded in plumbago crucible 6, it is the core component that solidifies purification, together with fixed support 9 is vertically fixed on insulation sleeve 7, and be fixedly installed in body of heater inside, ruhmkorff coil 8 is placed on insulation sleeve 7 peripheries, to silicon raw material, provide heat to make its fusing, insulation, powder discharging device 2 is placed on crucible top, by bracing frame 3, be fixed on body of heater 4 inside, powder discharging device is for providing high-purity silicon powder to bath surface, high-purity silicon powder is as nucleating agent, the silicon melt that surface impurity content is higher is solidified rapidly, play reverse induction and solidify the effect of purification, mechanical pump 14 and lobe pump 15 are positioned over outside body of heater 4, by vacuum pipe 16, connect, body of heater 4 inside are led in vacuum pipe 16 one end, for body of heater inside is vacuumized, make to solidify to purify and carry out under high vacuum.
Embodiment 2
Equipment described in employing embodiment 1 carries out oppositely induction and solidifies purifying polycrystalline silicon, first adopt ruhmkorff coil 8 that the silicon material in quartz crucible 5 is heated to 1450 ℃ and make it fusing formation silicon melt, afterwards the power of ruhmkorff coil 8 is turned down, startup water-cooled revolving bar 13 moves downward and draws ingot, silicon melt is solidified to top by quartz crucible 5 bottoms, when solidifying while reaching 80%, by water-cooled revolving bar 13 rotation quartz crucibles 5, open powder discharging device 2 is scattering in the upper strata silicon melt that foreign matter content is higher high-purity silicon powder simultaneously, high-purity silicon powder makes the rapid reverse solidification of upper strata silicon melt as nucleating agent, after having solidified, cut the part that upper strata reverse solidification obtains, the lower floor's ingot casting obtaining is HIGH-PURITY SILICON ingot casting.
The method that purifying polycrystalline silicon is solidified in above-mentioned a kind of reverse induction, the concrete steps that adopt are:
The first step pre-treatment: be 99.9% silicon raw material to the purity of adding quartz crucible volume 90% in quartz crucible 5, to packing purity in powder discharging device 2, be that 99.999% high-purity silicon powder is built bell 1, keep the stopping property in body of heater 2, with mechanical pump 14 and lobe pump 15, will in body of heater, be evacuated to 10Pa respectively;
Second step melt, draw ingot: opening power, start ruhmkorff coil 8, silicon material is heated to 1450 ℃, silicon material is melted completely, and be incubated 50min at 1450 ℃, control the temperature difference in melt simultaneously, open afterwards water-cooled revolving bar 13, make it to move downward with the speed of 1mm/min, drive is solidified attemperator and is declined and draw ingot with same speed, makes silicon melt to top, carry out directional freeze by quartz crucible 5 bottoms;
The 3rd step reverse solidification is purified: when silicon melt solidifies while reaching 80%, by water-cooled revolving bar 13 rotation quartz crucibles 5, open powder discharging device 2 simultaneously, high-purity silicon powder is dropped in melt, simultaneously by water-cooled revolving bar 13 rotation quartz crucibles 5, high-purity silicon powder is evenly distributed on silicon melt surface along with the rotation of quartz crucible 5, further reduction along with temperature, the high-purity silicon powder adding is as nucleating agent, make the rapid reverse solidification of silicon melt that foreign matter content is higher, after having solidified, cut the part that upper strata reverse solidification obtains, the lower floor's ingot casting obtaining is HIGH-PURITY SILICON ingot casting, its purity will reach 99.99%, yield rate reaches 80%.
Equipment described in employing embodiment 1 carries out oppositely induction and solidifies purifying polycrystalline silicon, first adopt ruhmkorff coil 8 that the silicon material in quartz crucible 5 is heated to 1500 ℃ and make it fusing formation silicon melt, afterwards the power of ruhmkorff coil 8 is turned down, startup water-cooled revolving bar 13 moves downward and draws ingot, silicon melt is solidified to top by quartz crucible 5 bottoms, when solidifying while reaching 85%, by water-cooled revolving bar 13 rotation quartz crucibles 5, open powder discharging device 2 simultaneously, high-purity silicon powder is scattering in the upper strata silicon melt that foreign matter content is higher, high-purity silicon powder makes the rapid reverse solidification of upper strata silicon melt as nucleating agent, after having solidified, cut the part that upper strata reverse solidification obtains, the lower floor's ingot casting obtaining is HIGH-PURITY SILICON ingot casting.
The method that purifying polycrystalline silicon is solidified in above-mentioned a kind of reverse induction, the concrete steps that adopt are:
The first step pre-treatment: be 99.93% silicon raw material to the purity of adding quartz crucible volume 95% in quartz crucible 5, to packing purity in powder discharging device 2, be that 99.9994% high-purity silicon powder is built bell 1, keep the stopping property in body of heater 2, with mechanical pump 14 and lobe pump 15, will in body of heater, be evacuated to 5Pa respectively;
Second step melt, draw ingot: opening power, start ruhmkorff coil 8, silicon material is heated to 1500 ℃, silicon material is melted completely, and be incubated 60min at 1500 ℃, control the temperature difference in melt simultaneously, open afterwards water-cooled revolving bar 13, make it to move downward with the speed of 0.4mm/min, drive is solidified attemperator and is declined and draw ingot with same speed, makes silicon melt to top, carry out directional freeze by quartz crucible 5 bottoms;
The 3rd step reverse solidification is purified: when silicon melt solidifies while reaching 85%, by water-cooled revolving bar 13 rotation quartz crucibles 5, open powder discharging device 2 simultaneously, high-purity silicon powder is dropped in silicon melt, simultaneously by water-cooled revolving bar 13 rotation quartz crucibles 5, high-purity silicon powder is evenly distributed on bath surface along with the rotation of quartz crucible 5, further reduction along with temperature, the high-purity silicon powder adding is as nucleating agent, make the rapid reverse solidification of silicon melt that foreign matter content is higher, after having solidified, cut the part that upper strata reverse solidification obtains, the lower floor's ingot casting obtaining is HIGH-PURITY SILICON ingot casting, its purity will reach 99.995%, yield rate reaches 90%.
Embodiment 4
Equipment described in employing embodiment 1 carries out oppositely induction and solidifies purifying polycrystalline silicon, first adopt ruhmkorff coil 8 that the silicon material in quartz crucible 5 is heated to 1550 ℃ and make it fusing formation silicon melt, afterwards the power of ruhmkorff coil 8 is turned down, startup water-cooled revolving bar 13 moves downward and draws ingot, silicon melt is solidified to top by quartz crucible 5 bottoms, when solidifying while reaching 90%, by water-cooled revolving bar 13 rotation quartz crucibles 5, open powder discharging device 2 simultaneously, high-purity silicon powder is scattering in the upper strata silicon melt that foreign matter content is higher, high-purity silicon powder makes the rapid reverse solidification of upper strata silicon melt as nucleating agent, after having solidified, cut the part that upper strata reverse solidification obtains, the lower floor's ingot casting obtaining is HIGH-PURITY SILICON ingot casting.
The method that purifying polycrystalline silicon is solidified in above-mentioned a kind of reverse induction, the concrete steps that adopt are:
The first step pre-treatment: be 99.95% silicon raw material to the purity of adding quartz crucible volume 100% in quartz crucible 5, to packing purity in powder discharging device 2, be that 99.9999% high-purity silicon powder is built bell 1, keep the stopping property in body of heater 2, with mechanical pump 14 and lobe pump 15, will in body of heater, be evacuated to 1Pa respectively;
Second step melt, draw ingot: opening power, start ruhmkorff coil 8, silicon material is heated to 1550 ℃, silicon material is melted completely, and be incubated 80min at 1550 ℃, control the temperature difference in melt simultaneously, open afterwards water-cooled revolving bar 13, make it to move downward with the speed of 0.1mm/min, drive is solidified attemperator and is declined and draw ingot with same speed, makes silicon melt to top, carry out directional freeze by quartz crucible 5 bottoms;
The 3rd step reverse solidification is purified: when silicon melt solidifies while reaching 90%, by water-cooled revolving bar 13 rotation quartz crucibles 5, open powder discharging device 2 simultaneously, high-purity silicon powder is dropped in silicon melt, simultaneously by water-cooled revolving bar 13 rotation quartz crucibles 5, high-purity silicon powder is evenly distributed on bath surface along with the rotation of quartz crucible 5, further reduction along with temperature, the high-purity silicon powder adding is as nucleating agent, make the rapid reverse solidification of silicon melt that foreign matter content is higher, after having solidified, cut the part that upper strata reverse solidification obtains, the lower floor's ingot casting obtaining is HIGH-PURITY SILICON ingot casting, its purity will reach 99.999%, yield rate reaches 95%.
Claims (9)
1. oppositely induce the method for solidifying purifying polycrystalline silicon for one kind, it is characterized in that: first adopt ruhmkorff coil (8) that the silicon material in quartz crucible (5) is heated to 1450～1550 ℃ and make it fusing formation silicon melt, starting afterwards water-cooled revolving bar (13) moves downward and draws ingot, silicon melt is solidified to top by quartz crucible (5) bottom, when solidifying while reaching 80%～90%, by water-cooled revolving bar (13) rotation quartz crucible (5), open powder discharging device (2) is scattering in the upper strata silicon melt that foreign matter content is higher high-purity silicon powder simultaneously, high-purity silicon powder makes the rapid reverse solidification of upper strata silicon melt as nucleating agent, after having solidified, cut the part that upper strata reverse solidification obtains, the lower floor's ingot casting obtaining is HIGH-PURITY SILICON ingot casting.
2. the method that purifying polycrystalline silicon is solidified in a kind of reverse induction according to claim 1, the concrete steps that adopt are:
The first step pre-treatment: be 99.9%～99.95% silicon raw material to the middle purity of adding quartz crucible volume 90%～100% of quartz crucible (5), in powder discharging device (2), pack high-purity silicon powder into, build bell (1), keep the stopping property in body of heater (4), use respectively mechanical pump (14) and lobe pump (15) in body of heater (4), to be evacuated to 1～10Pa;
Second step melt, draw ingot: opening power, start ruhmkorff coil (8), silicon material is heated to 1450～1550 ℃, silicon material is melted completely, and be incubated 50～80min at 1450～1550 ℃, control the temperature difference in melt simultaneously, open afterwards water-cooled revolving bar (13), make it to move downward with the speed of 0.1-1mm/min, drive is solidified attemperator and is declined and draw ingot with same speed, makes silicon melt to top, carry out directional freeze by quartz crucible (5) bottom;
The 3rd step reverse solidification is purified: when silicon melt solidifies while reaching 80%～90%, by water-cooled revolving bar (13) rotation quartz crucible (5), open powder discharging device (2) simultaneously, high-purity silicon powder is dropped in melt, high-purity silicon powder is evenly distributed on bath surface along with the rotation of quartz crucible (5), further reduction along with temperature, the high-purity silicon powder adding is as nucleating agent, make the rapid reverse solidification of silicon melt that foreign matter content is higher, after having solidified, cut the part that upper strata reverse solidification obtains, the lower floor's ingot casting obtaining is HIGH-PURITY SILICON ingot casting, its purity will reach 99.99%-99.999%.
3. the method that purifying polycrystalline silicon is solidified in arbitrary described a kind of reverse induction according to claim 1 or 2, is characterized in that: the purity of described high-purity silicon powder is 99.999%～99.9999%.
One kind oppositely induction solidify the equipment that the method for purifying polycrystalline silicon adopts, by bell (1), body of heater (4) and supporting base (11) form external structure, it is characterized in that: water-cooled revolving bar (13) is fixedly connected with water-cooled pallet (12) through body of heater (4) bottom, heating panel (10) is fixedly installed on water-cooled pallet (12), solidifying attemperator is positioned on heating panel (10), insulation sleeve (7) is placed on and solidifies attemperator periphery, insulation sleeve (7) is fixedly installed in body of heater (4) inwall by fixed support (9), ruhmkorff coil (8) is placed on outside insulation sleeve (7), powder discharging device (2) is fixed on body of heater (4) inside by bracing frame (3), and be positioned at and solidify directly over attemperator, mechanical pump (14) and lobe pump (15) are positioned over outside body of heater (4), by vacuum pipe (16), connect, body of heater (4) inside is led in vacuum pipe (16) one end.
5. the equipment that the method that purifying polycrystalline silicon is solidified in a kind of reverse induction according to claim 4 adopts, is characterized in that: described water-cooled revolving bar (13) is cylindric, built-in cooling water pipeline.
6. the equipment that the method that purifying polycrystalline silicon is solidified in a kind of reverse induction according to claim 4 adopts, is characterized in that: described water-cooled pallet (12) is discoid, built-in cooling water pipeline.
7. the equipment that the method that purifying polycrystalline silicon is solidified in a kind of reverse induction according to claim 4 adopts, is characterized in that: described heating panel (10), for discoid, is made of copper.
8. the equipment that the method that purifying polycrystalline silicon is solidified in a kind of reverse induction according to claim 4 adopts, it is characterized in that: described in solidify attemperator and at least by quartz crucible (5) and plumbago crucible (6), formed, adopt plumbago crucible (6) to be positioned on heating panel (10), within quartz crucible (5) is embedded in plumbago crucible (6).
9. the equipment that the method that purifying polycrystalline silicon is solidified in a kind of reverse induction according to claim 4 adopts, is characterized in that: what described insulation sleeve (7) was two ends uncovered is cylindric, by carbon fibre material, is made.
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| TWI619855B (en) * | 2016-12-21 | 2018-04-01 | Sun Wen Bin | Method for purifying high-purity silicon by fractionation |
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| CN108328618B (en) * | 2018-01-30 | 2021-02-09 | 青岛蓝光晶科新材料有限公司 | Method for separating hard inclusions in silicon by electromagnetic induction directional solidification |
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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 |
| CN102126725B (en) * | 2011-01-29 | 2012-12-19 | 大连隆田科技有限公司 | Method and equipment for purifying polycrystalline silicon by melting in electron beam shallow pool |
| CN102424388B (en) * | 2011-09-13 | 2013-02-27 | 山西纳克太阳能科技有限公司 | Method for removing metallic impurities in solar-grade polysilicon |
| CN202785671U (en) * | 2012-09-25 | 2013-03-13 | 青岛隆盛晶硅科技有限公司 | Device utilizing reverse induction solidification to purify polycrystalline silicon |
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