CN101428803B - Method and apparatus for producing high purity polysilicon with high-purity metal silicon purification - Google Patents
Method and apparatus for producing high purity polysilicon with high-purity metal silicon purification Download PDFInfo
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- CN101428803B CN101428803B CN2008102308045A CN200810230804A CN101428803B CN 101428803 B CN101428803 B CN 101428803B CN 2008102308045 A CN2008102308045 A CN 2008102308045A CN 200810230804 A CN200810230804 A CN 200810230804A CN 101428803 B CN101428803 B CN 101428803B
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- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 80
- 239000010703 silicon Substances 0.000 title claims abstract description 80
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 238000000034 method Methods 0.000 title claims abstract description 31
- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 31
- 229920005591 polysilicon Polymers 0.000 title claims abstract description 26
- 238000000746 purification Methods 0.000 title claims abstract description 20
- 239000002184 metal Substances 0.000 title claims description 22
- 229910052751 metal Inorganic materials 0.000 title claims description 22
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 93
- 239000010439 graphite Substances 0.000 claims abstract description 92
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 42
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229910052786 argon Inorganic materials 0.000 claims abstract description 18
- 238000004519 manufacturing process Methods 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 241000209456 Plumbago Species 0.000 claims description 49
- 238000009833 condensation Methods 0.000 claims description 18
- 230000005494 condensation Effects 0.000 claims description 18
- 239000007789 gas Substances 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000009413 insulation Methods 0.000 claims description 7
- 230000004223 radioprotective effect Effects 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 230000008569 process Effects 0.000 abstract description 8
- 239000002994 raw material Substances 0.000 abstract description 7
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 230000001681 protective effect Effects 0.000 abstract 1
- 239000012535 impurity Substances 0.000 description 19
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 6
- 239000000460 chlorine Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 230000009467 reduction Effects 0.000 description 4
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 4
- 239000005052 trichlorosilane Substances 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 239000011449 brick Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000004857 zone melting Methods 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000007770 graphite material Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
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- 239000010959 steel Substances 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
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- 238000010894 electron beam technology Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
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- 230000000630 rising effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229910021487 silica fume Inorganic materials 0.000 description 1
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Abstract
The invention relates to a method for preparing high-purity polysilicon from high-purity metallic silicon. Under the protective atmosphere of high-purity argon, a graphite crucible is taken as an anode, a vertical graphite electrode arranged in the middle of the graphite crucible is taken as a cathode, horizontal grates are staggered and arranged from top to bottom on the outer wall of the graphite electrode, the high-purity metallic silicon in the graphite crucible is heated to 1650-1800 DEG C and generates silicon vapor, the silicon vapor runs up to pass through the grates, and the high-purity polysilicon is collected after cooling treatment. Compared with the traditional purification process, the invention not only greatly reduces the purification technological process, but also has stable process and high efficiency, and reduces the raw material cost for solar batteries, so that obtained high-purify polysilicon has stable purify and good consistency. The production cost of purification equipment is low, no pollution is discharged in the production process, and the environmental protection is good.
Description
(1) technical field
The present invention relates to a kind of method and isolated plant of producing high purity polysilicon with high-purity metal silicon purification.
(2) background technology
At present, the production of polysilicon Technology mainly is divided into chemical method and physics method both at home and abroad.Chemical method is representative with improvement Siemens Method-closed loop hydrogen reduction of trichlorosilane mainly, this method is with chlorine and hydrogen synthesising hydrogen, hydrogenchloride again with industrial silica fume synthesizing trichlorosilane at a certain temperature, trichlorosilane is separated rectification and purification, and the trichlorosilane after the purification carries out the CVD reaction and produces high purity polycrystalline silicon in hydrogen reduction furnace.Polysilicon both domestic and external factory adopts this method to produce electronic-grade and solar-grade polysilicon, and the purity of the polysilicon of producing can reach 99.999999999% (11N), has satisfied the needs that the information industry unicircuit is made.As long as but that the purity of the needed polysilicon of solar cell reaches 99.9999% (6N) is above, unnecessary purity does not have too big practical significance for the transformation efficiency that improves solar cell.Therefore for producing solar-grade polysilicon, the production of improvement Siemens Method drops into too high, and complex process, energy consumption height, pollutes difficult control, this with reduce the solar cell cost-push and be not inconsistent.
In recent years, going up both at home and abroad and having formed exploitation is the solar-grade polysilicon production technique of representative with the physics method, and the mahjong physics method that adopts as the fast sky, Henan Science and Technology Ltd. is at the polysilicon product of producing 99.9999%～99.99999% in recent years in succession; Kawasaki, Japan system iron Co., Ltd., Nippon Steel Manufacturing Corp, JFE iron and steel etc. are also being obtained remarkable breakthrough aspect the physics fado crystal silicon production technology in succession.Physics method principal feature is that the production input is low, technology is simple than chemical method, production cost is low, product purity is lower, mainly comprises two kinds of metallurgy method and heavily doped scrap silicon method of purifications.As select purity preferably industrial silicon carry out the horizontal zone melting unidirectional solidification and become silicon ingot, remove in the silicon ingot after the metallic impurity accumulative part and outer matrix section, carry out coarse reduction and cleaning, melt at plasma body and to remove boron impurity in the stove, carry out horizontal zone melting second time unidirectional solidification again and become silicon ingot, remove metallic impurity accumulative part and outer matrix section in the zone melting and refining silicon ingot second time, after coarse reduction and cleaning, melt removal phosphorus and carbon impurity in the stove at electron beam, directly generate solar-grade polysilicon.But consider from reducing cost, simplify technological angle, develop more advanced production of polysilicon technology and be still the problem of being devoted to solve in the present industry.
(3) summary of the invention
The object of the present invention is to provide a kind of method of producing high purity polysilicon with high-purity metal silicon purification, can reduce production costs, simplify purifying technique.
The technical solution used in the present invention is as follows:
A kind of method of producing high purity polysilicon with high-purity metal silicon purification; in the protection atmosphere of high-purity argon gas; with the plumbago crucible be anodal, to be located at the vertical Graphite Electrodes of plumbago crucible intermediary be negative pole; on described plumbago crucible inwall and Graphite Electrodes outer wall, stagger up and down horizontal grate is set; high pure metal silicon in the heating plumbago crucible makes up the collection through the grid postcooling of silicon vapor obtain high purity polycrystalline silicon to 1650-1800 ℃ of generation silicon vapor.
Described silicon vapor is in 1450-1520 ℃ of cooling.
High-purity argon gas has been preheated to 1400-1500 ℃ when feeding.
The present invention also provides a kind of device of described producing high purity polysilicon with high-purity metal silicon purification, described device is a closed system, in closed system, be provided with plumbago crucible, be provided with vertical Graphite Electrodes in the middle of the plumbago crucible, plumbago crucible is provided with heating unit outward, the plumbago crucible top is provided with the silicon vapor condensation cover umbrella that confluxes, the silicon vapor condensation cover umbrella outer rim of confluxing has the liquid-state silicon collection container, staggering up and down on plumbago crucible inwall and the Graphite Electrodes outer wall is provided with horizontal grate, and plumbago crucible is connected with negative pole with the positive pole of power supply respectively with Graphite Electrodes.
The silicon vapor condensation cover umbrella that confluxes is arranged on the fixed link that the Graphite Electrodes top connects, and fixed link is connected and fixed on radioprotective isolates and cover; The liquid-state silicon collection container places the annular high purity graphite crucible of the support ring end face of plumbago crucible arranged outside for seat.
Heating unit is a heater coil, and heater coil is positioned at outside the support ring, is provided with backplate between heater coil and the support ring, and the heater coil outside is provided with the heat-insulation and heat-preservation material.
The present invention is not less than 99.99% high pure metal silicon with purity to carry out evaporative condenser, utilizes the protection atmosphere to separate with the electrical impurity of electrode pair to purify the preparation high purity polycrystalline silicon.Under the protection atmosphere of high-purity argon gas; high pure metal silicon in the plumbago crucible is heated into melt state; and at high temperature make silicon melt flash to the gas rising; when the grid of the Graphite Electrodes (negative pole) of silicon vapor gas by connecting power supply with when holding the grid of plumbago crucible (positive pole) of high pure metal silicon melt; because the grid of Graphite Electrodes is electronegative; the grid positively charged of plumbago crucible; the impurity that evaporates along with silicon vapor is under the effect of grid on the electrode; have electronegative impurity such as O; F; elements such as Cl leave silicon vapor and are attracted on the grid of crucible; have electropositive impurity such as P; B; Al; Sb; Ga; elements such as In leave on the grid that silicon vapor is attracted to graphite cathode; remove the silicon vapor cooling of electrical impurity; steam silicon becomes liquid silica drop, collects to obtain purity 99.9999%～99.99999% HIGH-PURITY SILICON crystal.
Concrete, the high pure metal silicon in the plumbago crucible can and make steam continue to rise by the coil heats fusing, and the current/voltage value by control coil can realize that system's full automatic control heats.
Carry out avoiding that impurity is to the influence of purification process in the air under the protection atmosphere of high-purity argon gas, purity of argon should be not less than 99.999%, and is concrete, can vacuumize total system earlier, and then charge into argon gas; Because in the process of applying argon gas, argon gas can absorb the part heat of silicon melt, makes the liquid-state silicon retrogradation, reduce the evaporation effect of liquid-state silicon, therefore preferred argon gas preheated before charging into closed system, and temperature is controlled at 1400～1500 ℃ and is advisable.Under argon shield atmosphere, the vaporator rate of partial impurities reduces in addition, and effusion impurity is difficult for diffusion but stays melt liquid surface, has suppressed the evaporation of partial impurities under melt state, as elements such as evaporation constant less B, Cu, Fe.
After collecting the silicon vapor of removing electrical impurity, cooling temperature needs only the temperature head of temperature existence with silicon melt, is convenient to collect so that silicon vapor is cooled to liquid silica drop, and cooling temperature is advisable with 1450 ℃～1520 ℃.
Grid on plumbago crucible and the Graphite Electrodes selects for use high purity graphite to make, and grid is intervally arranged, so that silicon vapor fully contacts the multilayer grid.
In order to strengthen the heat insulation effect of closed system, prevent that heat runs off, also heat-insulation and heat-preservation equipment can be set around device, isolate lid as the radioprotective that graphite material is set on silicon vapor collection device top, refractory brick is laid in the plumbago crucible bottom, and heat insulation carbon felt is set all around.
The present invention compares with traditional purifying technique, has not only significantly shortened the purifying technique flow process, and process stabilizing, efficient height, greatly reduces the raw materials cost of solar cell, and the high purity polycrystalline silicon purity that obtains is stable, high conformity; The low cost of manufacture of equipment for purifying does not have blowdown yet in the production process, environmental benefit is good.
(4) description of drawings
Fig. 1 is the device synoptic diagram of used producing high purity polysilicon with high-purity metal silicon purification among the embodiment.Each part description is as follows: lid is isolated in the 1-radioprotective; The 2-silicon vapor condensation cover umbrella that confluxes; The heat insulation carbon felt of 3-; The 4-plumbago crucible; The 5-Graphite Electrodes; 6-annular high purity graphite crucible; The 7-heater coil; The 8-support ring; 9-refractory brick; 10-graphite backplate; The 11-fixed link.
(5) embodiment:
Below with specific embodiment technical scheme of the present invention is described, but protection scope of the present invention is not limited thereto:
Embodiment 1
The device that adopts is as shown in Figure 1: comprise plumbago crucible 4, Graphite Electrodes 5, heater coil 7, silicon vapor condensation conflux cover umbrella 2 and annular high purity graphite crucible 6, stagger up and down on the vertical Graphite Electrodes outer wall of described plumbago crucible inwall and plumbago crucible intermediary and be provided with horizontal grate, the plumbago crucible top is provided with the silicon vapor condensation cover umbrella that confluxes, the silicon vapor condensation cover umbrella outer rim of confluxing has annular high purity graphite crucible, the silicon vapor condensation cover umbrella that confluxes is arranged on the fixed link 11 that the Graphite Electrodes top connects, and the radioprotective that fixed link is connected and fixed on graphite material is isolated and covered on 1; Annular high purity graphite crucible holder places on the end face of support ring 8 of the aluminum oxide of plumbago crucible arranged outside or zirconium white material.Refractory brick 9 is laid in the plumbago crucible bottom; Adopt heat insulation carbon felt 3 heat insulatings around the system; 8 of heater coil 7 and support rings are provided with graphite backplate 10.Plumbago crucible is connected with negative pole with the positive pole of power supply respectively with Graphite Electrodes.
Before the use,, charge into high-purity argon gas that purity is not less than 5N cleaning equipment inside repeatedly then, remove the impurity that device interior itself is had at first to total system extracting vacuum repeatedly.
Adding purity in the band grid plumbago crucible after cleaning is 99.99% high pure metal silicon raw material, closed system; Major impurity content in the raw material is Fe:16ppm (weight content, down together), P:4ppm, B:2.4ppm, Al:4.4ppm; System after the sealing vacuumizes once more, and control vacuum tightness is 10
-3Below the Torr, charge into then through 1420 ℃ of pre-warmed high-purity argon gas (purity is not less than 99.999%), and system is remained in the high-purity argon gas atmosphere, closed system air pressure is a little more than 1 standard atmospheric pressure.
To heater coil energising, regulate its electric current and magnitude of voltage and make heater coil the heating of gradient be arranged plumbago crucible and the silicon vapor condensation cover umbrella that confluxes; When the plumbago crucible temperature is heated to 1360 ℃, open the power supply of Graphite Electrodes and plumbago crucible electrode, make the Graphite Electrodes grid electronegative, plumbago crucible electrode grid positively charged.High pure metal silicon raw material begins fusing when surpassing 1420 ℃, and the outlet temperature of plumbago crucible is controlled at 1700 ℃; The vapour condensation temperature of covering umbrella of confluxing finally is controlled at 1480 ℃.Removing impurity by positive and negative electrode, is 99.99993% from the silicon vapor condensation HIGH-PURITY SILICON purity that the cover umbrella drips in the annular high purity graphite crucible of confluxing, and its foreign matter content is Fe:0.08ppm, P:0.10ppm, B:0.09ppm, Al:0.11ppm, C:4.6ppm, 0:1.8ppm, S:0.06ppm, Cl:0.038ppm, Cu:0.007ppm, In:0.0039ppm, Sn:0.0078ppm, Sb:0.0058ppm.
Embodiment 2
Treatment process before using appts and device use is with embodiment 1.
Adding purity is 99.99% high pure metal silicon raw material in plumbago crucible, its major impurity content F e:12ppm, and P:2.8ppm, B:1.5ppm, Al:3.7ppm, system is evacuated to vacuum tightness 10
-3Below the Torr, feeding closed system, to be preheated to 1450 ℃ purity be 99.999% argon gas, makes closed system air pressure a little more than 1 standard atmospheric pressure.When the plumbago crucible temperature is heated to 1370 ℃, open Graphite Electrodes and plumbago crucible power supply.The outlet temperature of plumbago crucible is controlled at 1750 ℃, and the silicon vapor condensation temperature of covering umbrella of confluxing finally is controlled at 1490 ℃.From the silicon vapor condensation HIGH-PURITY SILICON purity that drips in the annular high purity graphite crucible of cover umbrella of confluxing is 99.99996%, and its foreign matter content is Fe:0.072ppmt, P:0.09ppm, B:0.06ppm, Al:0.08ppm, C:4.2ppm, 0:1.6ppm, S:0.08ppm, Cl:0.036ppm, Cu:0.006ppm, In:0.0034ppm, Sn:0.0072ppm, Sb:0.0053ppm.
Embodiment 3
Treatment process before using appts and device use is with embodiment 1.
Adding purity is 99.99% metallic silicon raw material in plumbago crucible, and its major impurity content is Fe:9.8ppm, P:2.6ppm, and B:1.45ppm, Al:2.6ppm is evacuated to vacuum tightness 10
-3Below the Torr, add purity then and be 99.999% be preheated to 1480 ℃ argon gas, make closed system air pressure a little more than 1 standard atmospheric pressure.When the plumbago crucible temperature is heated to 1390 ℃, open the power supply of Graphite Electrodes and plumbago crucible.The outlet temperature of plumbago crucible is controlled at 1790 ℃, and the silicon vapor condensation temperature of covering umbrella of confluxing finally is controlled at 1510 ℃.From the silicon vapor condensation HIGH-PURITY SILICON purity that drips in the annular high purity graphite crucible of cover umbrella of confluxing is 99.99998%, and its foreign matter content is Fe:0.06ppmt, P:0.086ppm, B:0.055ppm, Al:0.076ppm, C:4.1ppmt, 0:1.48ppm, S:0.0553ppm, Cl:0.034ppm, Cu:0.0057ppm, In:0.0032ppm, Sn:0.0069ppm, Sb:0.0045ppm.
Claims (6)
1. the method for a producing high purity polysilicon with high-purity metal silicon purification; it is characterized in that: in the protection atmosphere of high-purity argon gas; with the plumbago crucible be anodal, to be located at the vertical Graphite Electrodes of plumbago crucible intermediary be negative pole; on described plumbago crucible inwall and Graphite Electrodes outer wall, stagger up and down horizontal grate is set; high pure metal silicon in the heating plumbago crucible makes up the collection through the grid postcooling of silicon vapor obtain high purity polycrystalline silicon to 1650-1800 ℃ of generation silicon vapor.
2. the method for producing high purity polysilicon with high-purity metal silicon purification as claimed in claim 1 is characterized in that, described silicon vapor is in 1450-1520 ℃ of cooling.
3. the method for producing high purity polysilicon with high-purity metal silicon purification as claimed in claim 1 or 2 is characterized in that, high-purity argon gas has been preheated to 1400-1500 ℃ when feeding.
4. device that is used for the described producing high purity polysilicon with high-purity metal silicon purification of claim 1, it is characterized in that, described device is a closed system, in closed system, be provided with plumbago crucible, be provided with vertical Graphite Electrodes in the middle of the plumbago crucible, plumbago crucible is provided with heating unit outward, the plumbago crucible top is provided with the silicon vapor condensation cover umbrella that confluxes, the silicon vapor condensation cover umbrella outer rim of confluxing has the liquid-state silicon collection container, staggering up and down on plumbago crucible inwall and the Graphite Electrodes outer wall is provided with horizontal grate, and plumbago crucible is connected with negative pole with the positive pole of power supply respectively with Graphite Electrodes.
5. the device that is used for producing high purity polysilicon with high-purity metal silicon purification as claimed in claim 4 is characterized in that, the silicon vapor condensation cover umbrella that confluxes is arranged on the fixed link that the Graphite Electrodes top connects, and fixed link is connected and fixed on radioprotective isolates and cover; The liquid-state silicon collection container places the annular high purity graphite crucible of the support ring end face of plumbago crucible arranged outside for seat.
6. the device that is used for producing high purity polysilicon with high-purity metal silicon purification as claimed in claim 5, it is characterized in that heating unit is a heater coil, heater coil is positioned at outside the support ring, be provided with backplate between heater coil and the support ring, the heater coil outside is provided with the heat-insulation and heat-preservation material.
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| CN2008102308045A CN101428803B (en) | 2008-11-10 | 2008-11-10 | Method and apparatus for producing high purity polysilicon with high-purity metal silicon purification |
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| CN101898763B (en) * | 2009-05-25 | 2012-09-05 | 高向瞳 | Method for preparing electric-field directional solidification purified polysilicon |
| US8562932B2 (en) * | 2009-08-21 | 2013-10-22 | Silicor Materials Inc. | Method of purifying silicon utilizing cascading process |
| CN101708850B (en) * | 2009-11-19 | 2011-09-14 | 大连理工大学 | Method and device for removing phosphorus and boron in polysilicon by continuous smelting |
| 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 |
| CN109023521A (en) * | 2018-08-29 | 2018-12-18 | 孟静 | The preparation method of solar cell module polysilicon chip |
| CN110668448A (en) * | 2018-12-12 | 2020-01-10 | 株洲诺天电热科技有限公司 | Single-side lateral horizontal collecting device of solid pure object electric heating equipment |
| CN110589836B (en) * | 2019-09-24 | 2021-03-26 | 东莞东阳光科研发有限公司 | Method and system for removing boron in industrial silicon refining |
| CN115074837A (en) * | 2022-06-10 | 2022-09-20 | 高伟 | Preparation equipment of rare earth metal single crystal |
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