CN201981011U - Coupled purifying equipment for removing phosphorus and metal in polycrystalline silicon by electron beam - Google Patents
Coupled purifying equipment for removing phosphorus and metal in polycrystalline silicon by electron beam Download PDFInfo
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- CN201981011U CN201981011U CN2011200308739U CN201120030873U CN201981011U CN 201981011 U CN201981011 U CN 201981011U CN 2011200308739 U CN2011200308739 U CN 2011200308739U CN 201120030873 U CN201120030873 U CN 201120030873U CN 201981011 U CN201981011 U CN 201981011U
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Abstract
The utility model belongs to the technical field of purifying polycrystalline silicon by the physical metallurgy technology, and relates to coupled purifying equipment for removing phosphorus and metal in polycrystalline silicon by an electron beam. In the equipment, vacuum equipment is formed by a vacuum cover, a vacuum furnace wall and a powder filling cover, the inner cavity of the vacuum equipment is a vacuum cavity, the upper part in the vacuum cavity is provided with a powder filling barrel, the bottom of the powder filling barrel is provided with a material outlet, the material outlet is assembled with an external-driving type powder baffle, the bottom of the material outlet of the powder filling barrel is provided with crucibles, the bottoms of the crucibles are provided with an ingot drawing mechanism, the ingot drawing mechanism is provided with a silicon ingot, an electric gun is arranged at the upper part of the vacuum cavity, and an electron beam flow aligns to the silicon ingot. The equipment disclosed by the utility model has the advantages that the structure of the equipment is simple; the technology of smelting powder silicon by the electron beam and the technology of directional solidification are simultaneously carried out, the electron beam is used for quickly removing phosphorus impurities, and the directional solidification is used for removing metal impurities with smaller segregation coefficient; the purify of the polycrystalline silicon is effectively improved, the use requirement of solar grade silicon can be reached, and the cost is low; and the equipment is suitable for batch production.
Description
Technical field
The utility model belongs to the technical field with physical metallurgy technology purifying polycrystalline silicon, particularly a kind of equipment for purifying that utilizes electron beam to remove phosphorus and metallic impurity in the polysilicon.
Background technology
Solar electrical energy generation becomes one of main path that realizes the low-carbon (LC) target as the important component part of renewable energy source, but be subjected to the restriction of the important source material-solar-grade polysilicon production cost of solar cell, the existing solar electrical energy generation installation amount of China is not high, the solar cell total installation of generating capacity only be 300MW by the year ends 2008 whole nations, no more than German 1 year newly-increased amount.Manufacturing cost that solar-grade polysilicon is high and complicated manufacturing process are the bottlenecks of restriction photovoltaic industry great development, have seriously hindered the popularization and the use of China's solar cell.Therefore the polysilicon technology of preparing of developing low-cost, high conversion efficiency is significant to the great development of China's photovoltaic industry,
At present, the preparation solar grade polycrystalline silicon material has formed large-scale production in the world wide, and main use technology route is the improvement Siemens Method.Siemens Method is to be raw material with hydrochloric acid (or hydrogen, chlorine) and metallurgical grade industrial silicon, by trichlorosilane, carries out the technology of hydrogen reduction.Be Siemens Method abroad now, and formed industry than proven technique.This method has been developed to the third generation, improves to the 4th generation now.First-generation Siemens Method is non-closed, and promptly Fan Ying by product hydrogen and trichlorosilane caused the very big wasting of resources.The third generation improvement Siemens process of widespread use has now realized complete loop production, and hydrogen, trichlorosilane silane and hydrochloric acid all are recycled, and scale is also at 1000 tons more than every year.But its comprehensive power consumption is up to 170kWh/kg, and produce and be discontinuity, can't in the production of Si, form and work continuously, and this method has been taked the thermal chemical vapor deposition that falls behind on the core link of flow process, the link of technical process is too much, one time transformation efficiency is low, causes the flow process time oversize, has increased material consumption, energy consumption cost.
Given this, try to explore to have with short production cycle, pollution is little, cost is low, the new preparation process method of the simple relatively solar-grade polysilicon of technology is very urgent, and metallurgy method is because possess above advantage, be considered to reduce effectively one of production of polysilicon cost techniques, become the focus that competitively research and develop countries in the world at present.Metallurgy method refers to process meanses such as directional freezes, removes metallic impurity; Adopt beam-plasma melting mode to remove boron; Adopt the electron beam melting mode to remove phosphorus, carbon, thereby obtain the method for the solar-grade polysilicon of low production cost.This method energy consumption is little, and the energy consumption of unit output is less than half of Siemens Method, and a plurality of countries such as Japan, the U.S., Norway are engaged in the research and development of metallurgy method now, wherein with the technology of Japanese JFE maturation the most, has dropped into industrialization production.The electron beam melting technology is that metallurgy method prepares one of important method in the solar-grade polysilicon, it is to utilize the processing method of the electron beam of high-energy-density as the melting thermal source, general electron beam melting method is after forming the molten bath by fusing buik silicon material, under the high temperature that electron beam produces, higher impurity such as the phosphorus of saturated vapor pressure is removed in surface evaporation, aluminium etc., and Impurity Distribution is very inhomogeneous in the buik silicon material, be unfavorable for the removal of impurity, and buik silicon material melting rear impurity is skewness still, simultaneously in numerous impurity of polysilicon, metal is very deleterious element, the uneven distribution of impurity and the existence of metallic impurity will produce adverse influence to the resistivity and the minority carrier lifetime of silicon materials, and then reduce the photoelectric transformation efficiency of solar cell.Electron beam melting powder silicon material still of no use is removed the coupling method of purification of phosphorus and metallic impurity in the polysilicon in known patent and the document.Known application number is 200810011631.8 patent of invention, utilize induction heating and electron beam to reach to remove the purpose of phosphorus and metallic impurity in the polysilicon, but the shortcoming of this method is additionally to have used induction heating, energy consumption is bigger, and what use is that the melting of buik silicon material is purified, and Impurity Distribution is inhomogeneous relatively.
Summary of the invention
The purpose of this utility model is to overcome above-mentioned not enough problem, a kind of electron beam dephosphorization is provided, removes the equipment of the coupling purifying polycrystalline silicon of metal, and is simple in structure, easy handling utilizes electron beam melting powder silicon material, removes phosphorus and metallic impurity simultaneously, purifying velocity is fast, the product purity height.
The technical scheme that the utility model is adopted for achieving the above object is: a kind of electron beam dephosphorization, remove the equipment of the coupling purifying polycrystalline silicon of metal, equipment adopts vacuum cover, vacuum furnace wall and dress powder lid to constitute vacuum apparatus, and the vacuum apparatus inner chamber is a vacuum chamber; The vacuum chamber internal upper part is equipped with the powder bucket, and dress powder bucket bottom has discharge port, and discharge port is equipped with the outer formula powder blocking plate that drives, crucible is equipped with in dress powder bucket discharge port bottom, and crucible bottom is equipped with ingot pulling mechanism, and silicon ingot is housed on the ingot pulling mechanism, electron beam gun is installed in vacuum chamber top, and electronic beam current is aimed at silicon ingot.
On the described vacuum apparatus vacuum extractor is installed, vacuum extractor adopts mechanical pump, lobe pump and diffusion pump.
Described ingot pulling mechanism adopts and draws the ingot support bar to be installed in the bottom of vacuum furnace wall, draws ingot support bar top that copper coin is installed, and graphite block is installed on the copper coin, places silicon ingot on the graphite block, draws in ingot support bar and the copper coin and offers coolant flow channel, and coolant flow channel is connected cooling source.
Described dress powder bucket top has dress powder lid, and dress powder lid is positioned on the vacuum furnace wall, and driving the formula powder blocking plate outward is L shaped powder blocking plate, and powder blocking plate one end is rotatably installed in the rotating mechanism, and rotating mechanism is installed in outside the vacuum furnace wall.
Described crucible is installed in the top of base for supporting, and base for supporting is installed in the bottom of vacuum furnace wall, and muff is installed on the base for supporting.
Unusual effect of the present utility model is a mode of taking electron beam melting powder silicon material and directional freeze simultaneously, remove foreign matter of phosphor fast with electron beam, remove with the metallic impurity that directional freeze is less with segregation coefficient, effectively improved the purity of polysilicon, reached the service requirements of solar energy level silicon.The electron beam melting purification techniques is one of important method of volatile impunty in the metallurgy method removal polysilicon, and it is a kind of melting purification process that utilizes the electron beam of high-energy-density as thermal source.In the process at the high-purity silicon ingot of beam bombardment top, the electronics of high-energy-density raises silicon material temperature after being converted into heat, thereby the silicon material is melted, under the effect of water-cooled copper annular crucible, form stable silicon molten bath, after silica flour fuses into the molten bath with certain flow, because specific surface area is bigger, burn-off rate is very fast, and volatile impunty phosphorus distributes more even with respect to the buik silicon material in silica flour, in the melting evaporative removal process after fusing, the removal speed of volatile impunty phosphorus is faster, and the distribution of residual impurity phosphorus simultaneously is also more even, and the resistivity size of the silicon ingot that obtains is also more even; In the evaporative removal foreign matter of phosphor, pull down ingot, directional freeze is carried out from the bottom to the top, produce the effect of segregation, the little metallic impurity of segregation coefficient are to the Liquid region enrichment, and the position of in the end solidifying is that assemble at the top of silicon ingot, and excision can be removed metallic impurity behind the top.The utility model refining effect is good, and is consistent, and technology is simple, the production efficiency height, and save energy, cost is low, is fit to produce in batches.
Description of drawings
Accompanying drawing 1 is a kind of electron beam dephosphorization, the equipment that removes the coupling purifying polycrystalline silicon of metal.
Among the figure, 1. the dress powder covers, 2. electron beam gun, 3. vacuum furnace wall, 4. vacuum chamber, 5. purging valve, 6. mechanical pump, 7. lobe pump, 8. diffusion pump, 9 base for supporting 10. draw the ingot support bar, 11. vacuum covers, 12. water-cooled copper plate, 13. graphite blocks, 14 muffs, 15. silicon ingots, 16. crucible, 17. molten baths, 18. silica flours, 19. powder blocking plate, 20. dress powder buckets, 21. rotating mechanisms.
Embodiment
Describe the utility model in detail below in conjunction with embodiment and accompanying drawing, but the utility model is not limited to specific embodiment.
Embodiment 1
A kind of electron beam dephosphorization as shown in Figure 1, remove metal the coupling purifying polycrystalline silicon equipment, equipment adopts vacuum cover 11, vacuum furnace wall 3 and dress powder lid 1 to constitute vacuum apparatus, the vacuum apparatus inner chamber is a vacuum chamber 4; The vacuum chamber internal upper part is equipped with the powder bucket, dress powder bucket top has dress powder lid, dress powder lid is positioned on the vacuum furnace wall, dress powder bucket bottom has discharge port, discharge port is equipped with the outer formula powder blocking plate that drives, driving the formula powder blocking plate outward is L shaped powder blocking plate, powder blocking plate one end is rotatably installed in the rotating mechanism, and rotating mechanism is installed in outside the vacuum furnace wall, and crucible is equipped with in dress powder bucket discharge port bottom, crucible 16 is installed in the top of base for supporting 9, base for supporting 9 is installed in the bottom of vacuum furnace wall 3, and muff 14 is installed on the base for supporting, and crucible bottom is equipped with ingot pulling mechanism, ingot pulling mechanism adopts and draws ingot support bar 10 to be installed in the bottom of vacuum furnace wall 3, draw ingot support bar 10 tops that copper coin 12 is installed, graphite block 13 is installed on the copper coin 12, place silicon ingot 15 on the graphite block, draw in ingot support bar and the copper coin and offer coolant flow channel, coolant flow channel is connected cooling source; Electron beam gun 2 is installed in vacuum chamber 4 tops, and electronic beam current is aimed at silicon ingot, and vacuum extractor is installed on the vacuum apparatus, and vacuum extractor adopts mechanical pump 6, lobe pump 7 and diffusion pump 8.
Adopt above-mentioned equipment to carry out the electron beam dephosphorization, remove the method for the coupling purifying polycrystalline silicon of metal, detailed process is:
The first step is got the raw materials ready: with phosphorus content 0.00004%, total metal content 0.0002% low-phosphorous, the low high-purity silicon ingot 15 of metal is put on the graphite block 8, low-phosphorous, the low high-purity silicon ingot of metal 15 tops are to be advisable with water-cooled copper annular crucible 16 upper surface levels, by rotating mechanism 21 powder blocking plate 19 is turned to dress powder bucket 20 bottom positions, to block the powder hole that falls, dress powder bucket 20 bottoms, open dress powder lid 1 and in dress powder bucket 20, add phosphorus content 0.003%, metallic impurity total content 0.01% high phosphorus, high metallic silicon power 18, high phosphorus, high metallic silicon power 18 Intake Quantitys are a little less than dress powder bucket 20 upper rim positions, close dress powder lid 1 and vacuum cover 11;
The second step pre-treatment: extracting vacuum, with mechanical pump 6, lobe pump 7 vacuum chamber 4 is extracted into rough vacuum 7Pa, with diffusion pump 8 vacuum chamber 4 is extracted into high vacuum 0.0018Pa again; By drawing ingot support bar 10 in water-cooled copper plate 12, to feed water coolant, with the temperature maintenance of water jacketed copper crucible at 44 ℃; Give electron beam gun 2 preheatings, it is 30kV that high pressure is set, and high pressure is closed high pressure after stablizing 5 minutes, and it is that 100mA carries out preheating that electron beam gun 2 lines are set, and preheating was closed electron beam gun 2 lines after 15 minutes;
The 3rd step: dephosphorization and metallic impurity: open the high pressure and the line of electron beam gun 2 simultaneously, after stablizing, with low-phosphorous, the low high-purity silicon ingot 15 of metal on the line bombardment graphite block 13 of 300mA, form stable molten bath 17 by electron beam gun 2; After forming stabilised bath 17, regulate electron beam gun 2 line sizes, make line maintain 400mA, powder blocking plate 19 is turned to the position of leaving dress powder bucket 20 bottoms by rotating mechanism 21, make high phosphorus, high metallic silicon power 18 fall into molten bath 17, simultaneously by drawing ingot support bar 10 to pull down ingot with certain speed; After waiting that powder finishes, at first close electron beam gun and stop to pull down ingot after 2,10 minutes, continued to vacuumize 30 minutes; Close diffusion pump 8 and continued to vacuumize 20 minutes, further close lobe pump 7 and mechanical pump 6 again, open purging valve 5 venting, open vacuum cover 11, take out silicon ingot from graphite block 5; Cut the impure more part in silicon ingot top at last, after testing, the content of the silicon ingot phosphorus that obtains is lower than 0.00004%, and the metallic impurity total content is lower than 0.0002%.
The mode of the utility model equipment while applying electronic bundle melting powder silicon material and directional freeze is removed phosphorus and metallic impurity in the polysilicon, removal effect is good, the efficient height, effectively use in the powder fusion process and melt fast and the Impurity Distribution advantage of uniform, integrated dephosphorization and remove the double effects of metal is fit to large-scale industrial production.
Claims (5)
1. an electron beam dephosphorization, remove metal the coupling purifying polycrystalline silicon equipment, it is characterized in that: equipment adopts vacuum cover, vacuum furnace wall and dress powder lid to constitute vacuum apparatus, and the vacuum apparatus inner chamber is a vacuum chamber; The vacuum chamber internal upper part is equipped with the powder bucket, and dress powder bucket bottom has discharge port, and discharge port is equipped with the outer formula powder blocking plate that drives, crucible is equipped with in dress powder bucket discharge port bottom, and crucible bottom is equipped with ingot pulling mechanism, and silicon ingot is housed on the ingot pulling mechanism, electron beam gun is installed in vacuum chamber top, and electronic beam current is aimed at silicon ingot.
2. a kind of electron beam dephosphorization according to claim 1, remove metal the coupling purifying polycrystalline silicon equipment, it is characterized in that: on the described vacuum apparatus vacuum extractor is installed, vacuum extractor adopts mechanical pump, lobe pump and diffusion pump.
3. a kind of electron beam dephosphorization according to claim 1, remove metal the coupling purifying polycrystalline silicon equipment, it is characterized in that: described ingot pulling mechanism adopts and draws the ingot support bar to be installed in the bottom of vacuum furnace wall, draw ingot support bar top that copper coin is installed, graphite block is installed on the copper coin, place silicon ingot on the graphite block, draw in ingot support bar and the copper coin and offer coolant flow channel, coolant flow channel is connected cooling source.
4. a kind of electron beam dephosphorization according to claim 1, remove metal the coupling purifying polycrystalline silicon equipment, it is characterized in that: described dress powder bucket top has dress powder lid, dress powder lid is positioned on the vacuum furnace wall, driving the formula powder blocking plate outward is L shaped powder blocking plate, powder blocking plate one end is rotatably installed in the rotating mechanism, and rotating mechanism is installed in outside the vacuum furnace wall.
5. a kind of electron beam dephosphorization according to claim 1, remove metal the coupling purifying polycrystalline silicon equipment, it is characterized in that: described crucible is installed in the top of base for supporting, base for supporting is installed in the bottom of vacuum furnace wall, and muff is installed on the base for supporting.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011200308739U CN201981011U (en) | 2011-01-29 | 2011-01-29 | Coupled purifying equipment for removing phosphorus and metal in polycrystalline silicon by electron beam |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011200308739U CN201981011U (en) | 2011-01-29 | 2011-01-29 | Coupled purifying equipment for removing phosphorus and metal in polycrystalline silicon by electron beam |
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| CN201981011U true CN201981011U (en) | 2011-09-21 |
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| CN2011200308739U Expired - Fee Related CN201981011U (en) | 2011-01-29 | 2011-01-29 | Coupled purifying equipment for removing phosphorus and metal in polycrystalline silicon by electron beam |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102120578A (en) * | 2011-01-29 | 2011-07-13 | 大连隆田科技有限公司 | Method and device for coupling and purifying polysilicon and removing phosphorus and metal with electron beams |
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2011
- 2011-01-29 CN CN2011200308739U patent/CN201981011U/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102120578A (en) * | 2011-01-29 | 2011-07-13 | 大连隆田科技有限公司 | Method and device for coupling and purifying polysilicon and removing phosphorus and metal with electron beams |
| CN102120578B (en) * | 2011-01-29 | 2012-10-03 | 大连隆田科技有限公司 | Method and device for coupling and purifying polysilicon and removing phosphorus and metal with electron beams |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20110921 Termination date: 20130129 |
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| CF01 | Termination of patent right due to non-payment of annual fee |