CN102849743A - 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 the metallurgy purification technical field, particularly a kind of method of solidifying purification of oppositely inducing also relates to its equipment in addition.
Background technology
At present, China has become world energy sources production and consumption big country, but the energy expenditure level is also very low per capita.Along with development economic and society, China's energy demand is with sustainable growth, for present 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's newly-increased grid-connected photovoltaic power generation in 2010 530000 kW that install, the 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 about 130,000 kW that install.The newly-increased installation in 2010 of photovoltaic generation market, the whole world is estimated to increase on year-on-year basis to surpass 120%, reaches more than 1,700 ten thousand kW, drives China's photovoltaic industry size and enlarges rapidly.
The development of photovoltaic industry depends on the purification to the silicon raw material.In the process that the silicon raw material is purified, there is a key, requisite link, exactly the silicon raw material is carried out directional freeze and purify, used directional solidification technique is widely used in field of metallurgy purification.Utilize the segregation coefficient between the silicon and impurity in the silicon raw material to have these characteristics of larger difference, in process of setting, the silicon liquid of crucible bottom at first begins to solidify, for reaching the fractional condensation balance, the impurity that segregation coefficient is little out is gathered in liquid state to the continuous separation by diffusion of liquid state from the silicon that solidifies, carry out along with solidifying constantly, the concentration of impurity in liquid state is more and more higher, solidify at last lower on the top of ingot casting, solidify and under comparatively high temps, be incubated for some time after finishing, make each composition fully spread to reach the fractional condensation balance, the end that foreign matter content is higher is removed at last, the polycrystalline silicon ingot casting that obtains 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, so that silicon purity is along with the on the contrary gradually reduction of prolongation of soaking time, this has affected refining effect, and in this case, the afterbody waste material of excision is up to 25% ~ 35%, and namely yield rate only is 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, a kind of method of solidifying purifying polycrystalline silicon of oppositely inducing is provided, the method uses silica flour as nucleating agent, impurity is fixed on 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 provides a kind of equipment that solidifies purifying polycrystalline silicon of oppositely inducing, this device structure is simple, easy handling, and effectively the purpose of solidifying purification is oppositely induced in realization.
The technical scheme that adopts for achieving the above object is: a kind of method of solidifying purifying polycrystalline silicon of oppositely inducing, at first adopt ruhmkorff coil that the silicon material in the quartz crucible is heated to 1450 ~ 1550 ℃ and make it fusing formation silicon melt, starting afterwards the water-cooled revolving bar moves downward and draws ingot, silicon melt is solidified to the top by the quartz crucible bottom, when solidifying when reaching 80% ~ 90%, by water-cooled revolving bar rotation quartz crucible, opening simultaneously powder discharging device is scattering in the higher upper strata silicon melt of foreign matter content high-purity silicon powder, high-purity silicon powder makes the rapid reverse solidification of upper strata silicon melt as nucleating agent, cut the part that the upper strata reverse solidification obtains wait solidifying after finishing, the lower floor's ingot casting that obtains is the HIGH-PURITY SILICON ingot casting.
Described a kind of method of solidifying purifying polycrystalline silicon of oppositely inducing, the concrete steps that adopt are:
The first step pre-treatment: the purity of adding quartz crucible volume 90% ~ 100% in the quartz crucible is 99.9% ~ 99.95% silicon raw material, the high-purity silicon powder of packing in the powder discharging device is built bell, keep the stopping property in the body of heater, will be evacuated to 1 ~ 10Pa in the body of heater with mechanical pump and lobe pump respectively;
The second step melt, draw ingot: opening power, start ruhmkorff coil, the silicon material is heated to 1450 ~ 1550 ℃, the silicon material is melted fully, and at 1450 ~ 1550 ℃ of lower insulation 50 ~ 80min, control simultaneously the temperature difference in the melt, open afterwards the water-cooled revolving bar, make it to move downward with the speed of 0.1-1mm/min, drive is solidified attemperator and is drawn ingot with same speed decline, makes silicon melt carry out directional freeze to the top by the quartz crucible bottom;
The 3rd step reverse solidification is purified: when silicon melt solidifies when reaching 80% ~ 90%, by water-cooled revolving bar rotation quartz crucible, open simultaneously powder discharging device, high-purity silicon powder is dropped in the 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 that adds is as nucleating agent, make the rapid reverse solidification of the higher silicon melt of foreign matter content, cut the part that the upper strata reverse solidification obtains wait solidifying after finishing, the lower floor's ingot casting that obtains is the HIGH-PURITY SILICON ingot casting, and its purity will reach 99.99%-99.999%, and yield rate reaches 80-95%.
The purity of described high-purity silicon powder is 99.999% ~ 99.9999%.
A kind of equipment of oppositely inducing the method for solidifying purifying polycrystalline silicon to adopt, by bell, body of heater and supporting base form external structure, it is characterized in that: the water-cooled revolving bar passes bottom of furnace body and is fixedly connected with the water-cooled pallet, heating panel is fixedly installed on the water-cooled pallet, solidifying attemperator is positioned on the heating panel, the muff jacket casing is in solidifying the attemperator periphery, the insulation sleeve is fixedly installed in inboard wall of furnace body by fixed support, ruhmkorff coil is placed in outside the insulation sleeve, powder discharging device is fixed in body of heater inside by bracing frame, and be positioned at and solidify directly over the attemperator, mechanical pump and lobe pump are positioned over outside the body of heater, connect by vacuum pipe, vacuum pipe one end leads to body of heater inside.
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 comprised of quartz crucible and plumbago crucible at least, adopts plumbago crucible to be positioned on the heating panel, and quartz crucible is embedded within the 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 evenly is scattering into the silicon melt surface, silica flour solidifies rapidly the higher upper strata silicon melt of foreign matter content as nucleating agent, establishment the impurity that content is higher in the silicon melt of upper strata in insulating process to the diffusion of the low concentration region that solidified, reached and oppositely induced the purpose of solidifying purifying polycrystalline silicon, it is good, simple to operate that this equipment has a refining effect, the advantage that controllability is strong.
Description of drawings
Fig. 1. a kind of device structure synoptic diagram that solidifies purifying polycrystalline silicon of oppositely inducing
Among the figure, 1, bell, 2, powder discharging device, 3, bracing frame, 4, body of heater, 5, quartz crucible, 6, plumbago crucible, 7, the insulation sleeve, 8, ruhmkorff coil, 9, fixed support, 10, heating panel, 11, supporting base, 12, water-cooled pallet, 13, the water-cooled revolving bar, 14, mechanical pump, 15, lobe pump, 16, vacuum pipe.
Embodiment
Describe the present invention in detail below in conjunction with specific embodiments and the drawings, but the present invention is not limited to specific embodiment.
Embodiment 1
A kind of equipment that solidifies purifying polycrystalline silicon of oppositely inducing as shown in Figure 1, by bell 1, body of heater 4 and supporting base 11 form external structure, water-cooled revolving bar 13 passes body of heater 4 bottoms and is fixedly connected with water-cooled pallet 12, the purpose of water-cooled revolving bar 13 is to play to drive the crucible rotation in purification process, powder falling is evenly trickled down at bath surface, crucible is moved downward with given pace, 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 the crucible top to forming a thermograde between the bottom, be convenient to solidifying of crucible bottom melt, form ingot casting, solidifying attemperator is positioned on the heating panel 10, solidifying attemperator is comprised of quartz crucible 5 and plumbago crucible 6 at least, adopt plumbago crucible 6 to be positioned on the heating panel 10, quartz crucible 5 is embedded within the plumbago crucible 6, it is the core component that solidifies purification, fixed support 9 and insulation sleeve 7 are vertically fixed on together, and be fixedly installed in body of heater inside, ruhmkorff coil 8 is placed in insulation sleeve 7 peripheries, provide heat to make its fusing to the silicon raw material, insulation, powder discharging device 2 is placed on the crucible top, be fixed in body of heater 4 inside by bracing frame 3, powder discharging device is used for providing high-purity silicon powder to bath surface, high-purity silicon powder is as nucleating agent, the higher silicon melt of surface impurity content is solidified rapidly, play and oppositely induce the effect of solidifying purification, mechanical pump 14 and lobe pump 15 are positioned over outside the body of heater 4, connect by vacuum pipe 16, and vacuum pipe 16 1 ends lead to body of heater 4 inside, be used for body of heater inside is vacuumized, make that solidifying purifies carries out under high vacuum.
Embodiment 2
Adopt embodiment 1 described equipment oppositely to induce and solidify purifying polycrystalline silicon, at first adopt ruhmkorff coil 8 that the silicon material in the 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 the top by quartz crucible 5 bottoms, when solidifying when reaching 80%, by water-cooled revolving bar 13 rotation quartz crucibles 5, opening simultaneously powder discharging device 2 is scattering in the higher upper strata silicon melt of foreign matter content high-purity silicon powder, high-purity silicon powder makes the rapid reverse solidification of upper strata silicon melt as nucleating agent, cut the part that the upper strata reverse solidification obtains wait solidifying after finishing, the lower floor's ingot casting that obtains is the HIGH-PURITY SILICON ingot casting.
Above-mentioned a kind of method of solidifying purifying polycrystalline silicon of oppositely inducing, the concrete steps that adopt are:
The first step pre-treatment: the purity of adding quartz crucible volume 90% in the quartz crucible 5 is 99.9% silicon raw material, the purity of packing in the powder discharging device 2 is that 99.999% high-purity silicon powder is built bell 1, keep the stopping property in the body of heater 2, will be evacuated to 10Pa in the body of heater with mechanical pump 14 and lobe pump 15 respectively;
The second step melt, draw ingot: opening power, start ruhmkorff coil 8, the silicon material is heated to 1450 ℃, the silicon material is melted fully, and at 1450 ℃ of lower insulation 50min, control simultaneously the temperature difference in the melt, open afterwards water-cooled revolving bar 13, make it to move downward with the speed of 1mm/min, drive is solidified attemperator and is drawn ingot with same speed decline, makes silicon melt carry out directional freeze to the top by quartz crucible 5 bottoms;
The 3rd step reverse solidification is purified: when silicon melt solidifies when reaching 80%, by water-cooled revolving bar 13 rotation quartz crucibles 5, open simultaneously powder discharging device 2, high-purity silicon powder is dropped in the melt, simultaneously by water-cooled revolving bar 13 rotation quartz crucibles 5, high-purity silicon powder is evenly distributed on the silicon melt surface along with the rotation of quartz crucible 5, further reduction along with temperature, the high-purity silicon powder that adds is as nucleating agent, make the rapid reverse solidification of the higher silicon melt of foreign matter content, cut the part that the upper strata reverse solidification obtains wait solidifying after finishing, the lower floor's ingot casting that obtains is the HIGH-PURITY SILICON ingot casting, its purity will reach 99.99%, and yield rate reaches 80%.
Embodiment 3
Adopt embodiment 1 described equipment oppositely to induce and solidify purifying polycrystalline silicon, at first adopt ruhmkorff coil 8 that the silicon material in the 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 the top by quartz crucible 5 bottoms, when solidifying when reaching 85%, by water-cooled revolving bar 13 rotation quartz crucibles 5, open simultaneously powder discharging device 2, high-purity silicon powder is scattering in the higher upper strata silicon melt of foreign matter content, high-purity silicon powder makes the rapid reverse solidification of upper strata silicon melt as nucleating agent, cut the part that the upper strata reverse solidification obtains wait solidifying after finishing, the lower floor's ingot casting that obtains is the HIGH-PURITY SILICON ingot casting.
Above-mentioned a kind of method of solidifying purifying polycrystalline silicon of oppositely inducing, the concrete steps that adopt are:
The first step pre-treatment: the purity of adding quartz crucible volume 95% in the quartz crucible 5 is 99.93% silicon raw material, the purity of packing in the powder discharging device 2 is that 99.9994% high-purity silicon powder is built bell 1, keep the stopping property in the body of heater 2, will be evacuated to 5Pa in the body of heater with mechanical pump 14 and lobe pump 15 respectively;
The second step melt, draw ingot: opening power, start ruhmkorff coil 8, the silicon material is heated to 1500 ℃, the silicon material is melted fully, and at 1500 ℃ of lower insulation 60min, control simultaneously the temperature difference in the melt, 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 drawn ingot with same speed decline, makes silicon melt carry out directional freeze to the top by quartz crucible 5 bottoms;
The 3rd step reverse solidification is purified: when silicon melt solidifies when reaching 85%, by water-cooled revolving bar 13 rotation quartz crucibles 5, open simultaneously powder discharging device 2, high-purity silicon powder is dropped in the 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 that adds is as nucleating agent, make the rapid reverse solidification of the higher silicon melt of foreign matter content, cut the part that the upper strata reverse solidification obtains wait solidifying after finishing, the lower floor's ingot casting that obtains is the HIGH-PURITY SILICON ingot casting, its purity will reach 99.995%, and yield rate reaches 90%.
Embodiment 4
Adopt embodiment 1 described equipment oppositely to induce and solidify purifying polycrystalline silicon, at first adopt ruhmkorff coil 8 that the silicon material in the 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 the top by quartz crucible 5 bottoms, when solidifying when reaching 90%, by water-cooled revolving bar 13 rotation quartz crucibles 5, open simultaneously powder discharging device 2, high-purity silicon powder is scattering in the higher upper strata silicon melt of foreign matter content, high-purity silicon powder makes the rapid reverse solidification of upper strata silicon melt as nucleating agent, cut the part that the upper strata reverse solidification obtains wait solidifying after finishing, the lower floor's ingot casting that obtains is the HIGH-PURITY SILICON ingot casting.
Above-mentioned a kind of method of solidifying purifying polycrystalline silicon of oppositely inducing, the concrete steps that adopt are:
The first step pre-treatment: the purity of adding quartz crucible volume 100% in the quartz crucible 5 is 99.95% silicon raw material, the purity of packing in the powder discharging device 2 is that 99.9999% high-purity silicon powder is built bell 1, keep the stopping property in the body of heater 2, will be evacuated to 1Pa in the body of heater with mechanical pump 14 and lobe pump 15 respectively;
The second step melt, draw ingot: opening power, start ruhmkorff coil 8, the silicon material is heated to 1550 ℃, the silicon material is melted fully, and at 1550 ℃ of lower insulation 80min, control simultaneously the temperature difference in the melt, 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 drawn ingot with same speed decline, makes silicon melt carry out directional freeze to the top by quartz crucible 5 bottoms;
The 3rd step reverse solidification is purified: when silicon melt solidifies when reaching 90%, by water-cooled revolving bar 13 rotation quartz crucibles 5, open simultaneously powder discharging device 2, high-purity silicon powder is dropped in the 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 that adds is as nucleating agent, make the rapid reverse solidification of the higher silicon melt of foreign matter content, cut the part that the upper strata reverse solidification obtains wait solidifying after finishing, the lower floor's ingot casting that obtains is the HIGH-PURITY SILICON ingot casting, its purity will reach 99.999%, and yield rate reaches 95%.
Claims (9)
1. oppositely induce the method for solidifying purifying polycrystalline silicon for one kind, it is characterized in that: at first the silicon material in the quartz crucible (5) is heated to 1450 ~ 1550 ℃ and makes it fusing formation silicon melt, starting afterwards water-cooled revolving bar (13) moves downward and draws ingot, silicon melt is solidified to the top by quartz crucible (5) bottom, when solidifying when reaching 80% ~ 90%, by water-cooled revolving bar (13) rotation quartz crucible (5), opening simultaneously powder discharging device (2) is scattering in the higher upper strata silicon melt of foreign matter content high-purity silicon powder, high-purity silicon powder makes the rapid reverse solidification of upper strata silicon melt as nucleating agent, cut the part that the upper strata reverse solidification obtains wait solidifying after finishing, the lower floor's ingot casting that obtains is the HIGH-PURITY SILICON ingot casting.
2. a kind of method of solidifying purifying polycrystalline silicon of oppositely inducing according to claim 1, the concrete steps that adopt are:
The first step pre-treatment: the purity to the middle interpolation of quartz crucible (5) quartz crucible volume 90% ~ 100% is 99.9% ~ 99.95% silicon raw material, the high-purity silicon powder of packing in the powder discharging device (2), build bell (1), keep the stopping property in the body of heater (2), use respectively mechanical pump (14) and lobe pump (15) to be evacuated to 1 ~ 10Pa in the body of heater;
The second step melt, draw ingot: opening power, start ruhmkorff coil (8), the silicon material is heated to 1450 ~ 1550 ℃, the silicon material is melted fully, and at 1450 ~ 1550 ℃ of lower insulation 50 ~ 80min, control simultaneously the temperature difference in the melt, 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 drawn ingot with same speed decline, makes silicon melt carry out directional freeze to the top by quartz crucible (5) bottom;
The 3rd step reverse solidification is purified: when silicon melt solidifies when reaching 80% ~ 90%, by water-cooled revolving bar (13) rotation quartz crucible (5), open simultaneously powder discharging device (2), high-purity silicon powder is dropped in the 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 that adds is as nucleating agent, make the rapid reverse solidification of the higher silicon melt of foreign matter content, cut the part that the upper strata reverse solidification obtains wait solidifying after finishing, the lower floor's ingot casting that obtains is the HIGH-PURITY SILICON ingot casting, and its purity will reach 99.99%-99.999%.
3. arbitrary described a kind of method of solidifying purifying polycrystalline silicon of oppositely inducing according to claim 1 and 2, it is characterized in that: the purity of described high-purity silicon powder is 99.999% ~ 99.9999%.
4. equipment of oppositely inducing the method for solidifying purifying polycrystalline silicon to adopt, by bell (1), body of heater (4) and supporting base (11) form external structure, it is characterized in that: water-cooled revolving bar (13) passes body of heater (4) bottom and is fixedly connected with water-cooled pallet (12), heating panel (10) is fixedly installed on the water-cooled pallet (12), solidifying attemperator is positioned on the heating panel (10), insulation sleeve (7) is placed in and solidifies the attemperator periphery, insulation sleeve (7) is fixedly installed in body of heater (4) inwall by fixed support (9), ruhmkorff coil (8) is placed in outside the insulation sleeve (7), powder discharging device (2) is fixed in body of heater (4) inside by bracing frame (3), and be positioned at and solidify directly over the attemperator, mechanical pump (14) and lobe pump (15) are positioned over outside the body of heater (4), connect by vacuum pipe (16), vacuum pipe (16) one ends lead to body of heater (4) inside.
5. a kind of equipment of oppositely inducing the method for solidifying purifying polycrystalline silicon to adopt according to claim 4 is characterized in that: described water-cooled revolving bar (13) is for cylindric, built-in cooling water pipeline.
6. a kind of equipment of oppositely inducing the method for solidifying purifying polycrystalline silicon to adopt according to claim 4 is characterized in that: described water-cooled pallet (12) is for discoid, built-in cooling water pipeline.
According to claim 4 a kind of oppositely induce solidify purifying polycrystalline silicon the equipment that adopts of method, it is characterized in that: described heating panel (10) is discoid copper heating panel.
8. a kind of equipment of oppositely inducing the method for solidifying purifying polycrystalline silicon to adopt according to claim 4, it is characterized in that: the described attemperator that solidifies is comprised of quartz crucible (5) and plumbago crucible (6) at least, adopt plumbago crucible (6) to be positioned on the heating panel (10), quartz crucible (5) is embedded within the plumbago crucible (6).
9. a kind of equipment of oppositely inducing the method for solidifying purifying polycrystalline silicon to adopt according to claim 4, it is characterized in that: described insulation sleeve (7) is the cylindric carbon fibre material insulation sleeve of two ends uncovered.
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| CN103266350A (en) * | 2013-05-31 | 2013-08-28 | 大连理工大学 | Vacuum solid-liquid separation method and device for polycrystalline silicon ingot |
| CN103266349B (en) * | 2013-05-31 | 2015-07-15 | 大连理工大学 | High-purity hollow silicon material, as well as polycrystalline silicon and ingot silicon vacuum solid-liquid separation method and equipment |
| CN103266350B (en) * | 2013-05-31 | 2015-08-12 | 大连理工大学 | Vacuum solid-liquid separation and separating device |
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| CN103466630A (en) * | 2013-09-26 | 2013-12-25 | 青岛隆盛晶硅科技有限公司 | Polycrystalline silicon directional solidifying method and device capable of improving impurity removal effect |
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| CN103553049B (en) * | 2013-10-18 | 2015-09-02 | 青岛隆盛晶硅科技有限公司 | The medium melting being applied to polycrystalline silicon purifying is connected preliminary directional solidification processes |
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| CN103553049A (en) * | 2013-10-18 | 2014-02-05 | 青岛隆盛晶硅科技有限公司 | Medium smelting cohesion primary directional solidification process applied to purifying polycrystalline silicon |
| CN103539125B (en) * | 2013-10-18 | 2015-09-02 | 青岛隆盛晶硅科技有限公司 | Medium melting is connected the method for purifying polycrystalline silicon with preliminary directional freeze |
| CN103539126A (en) * | 2013-10-30 | 2014-01-29 | 大连理工大学 | Rapid freezing method of polycrystalline silicon |
| CN103539126B (en) * | 2013-10-30 | 2016-04-13 | 大连理工大学 | A kind of polysilicon quick setting method |
| CN104556049A (en) * | 2014-12-25 | 2015-04-29 | 大连理工大学 | Equipment and method for increasing purifying yield in polycrystalline silicon orientated solidification |
| CN104528733A (en) * | 2014-12-25 | 2015-04-22 | 大连理工大学 | Device and method for separating high-metal-impurity region from cast ingot |
| CN104528733B (en) * | 2014-12-25 | 2016-06-01 | 大连理工大学 | A kind of equipment and method being separated high metallic impurity district for ingot casting |
| CN108328618A (en) * | 2018-01-30 | 2018-07-27 | 青岛蓝光晶科新材料有限公司 | A kind of method of hard inclusions in electromagnetic induction directional solidification divided silicon |
| 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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