CN102408112A - Method and equipment for purification of polysilicon by using electron beam melting under action of high purity silicon substrate - Google Patents
Method and equipment for purification of polysilicon by using electron beam melting under action of high purity silicon substrate Download PDFInfo
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Abstract
The invention belongs to the technical field of purification of polysilicon by using the technology of physical metallurgy. A method for purification of polysilicon by using electron beam melting under the action of a high purity silicon substrate comprises the following steps: step 1, preparing materials and carrying out pretreatment; step 2, forming the high purity silicon substrate, that is, unlatching an electron beam with a beam current of 200 to 500 mA to fully fuse a high purity silicon material, allowing the beam current to slowly decrease to 0, i.e., to form high purity polysilicon ingots in a water cooled crucible, and adjusting the beam current of the electron beam to be 150 to 300 mA to fuse the high purity polysilicon ingots so as to obtain a layer of the high purity silicon substrate formed in 2 to 5 min; step 3, carrying out melting and purification, that is, allowing a high phosphorus silicon material to slowly fall into a molten pool, increasing the beam current to 300 to 700 mA, fusing the high phosphorus silicon material to obtain high phosphorus silicon liquid, allowing the high phosphorus silicon liquid to flow into the crucible from a diversion mouth after removal of impurity phosphorus so as to obtain low phosphorus silicon liquid and solidifying the low phosphorus silicon liquid to obtain low phosphorus polysilicon ingots. The method provided in the invention has the advantages of a good purification effect, a simple process, conserved energy, reduced pollution and suitability for mass production; and equipment provided in the invention has the advantages of a simple structure, unique design, simple operation, low cost and capacity of realizing continuous smelting.
Description
Technical field
The invention belongs to technical field, carry out the electron beam melting purifying polycrystalline silicon under the effect of particularly a kind of HIGH-PURITY SILICON substrate, remove the method for the foreign matter of phosphor in the polysilicon with physical metallurgy technology purifying polycrystalline silicon; The invention still further relates to its equipment in addition.
Background technology
Solar cell can be an electric energy with conversion of solar energy, and in conventional energy resources today in short supply, sun power has huge using value.Solar grade polycrystalline silicon material is one of important raw and processed materials of preparation solar battery sheet.At present, preparation polycrystalline silicon used for solar battery material has formed large-scale production in the world wide, and main technological route has:
(1) 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 the by product hydrogen and the trichlorosilane of reaction have 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 produces and be discontinuity, can't in the production of Si, form and work continuously.
(2) silane thermal decomposition process: be with silicofluoric acid (H
2SiF
6), sodium, aluminium, hydrogen is that main raw material(s) is produced silane (SiH
4), the technology of producing polysilicon then through thermolysis.This method is based on chemical technology, and energy consumption is bigger, compares no clear superiority with the siemens method.
(3) fluidized bed method: be with SiCl
4(or SiF
4) and metallurgical grade silicon be raw material, produce the technology of polysilicon.The granular polycrystalline silicon Process is typically a kind of in the fluidized bed operational path.But the technological line of this technology is just in the debug phase.
(4) metallurgy method:, remove metallic impurity with process meanses such as directional freezes; Adopt beam-plasma melting mode to remove boron; Adopt the electron beam melting mode to remove phosphorus, carbon, thereby obtain the solar-grade polysilicon of low production cost.This method energy consumption is little, and the energy consumption of unit output is half the less than 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, and wherein the technology with Japanese JFE is the most ripe, has dropped into industrialization production.
In numerous methods that prepare silicon materials, can invested in plant production have only improvement Siemens Method, silane thermal decomposition process, metallurgy method.But the facility investment of improvement Siemens Method and silane thermal decomposition process is big, cost is high, seriously polluted, complex process; The popularization that is unfavorable for solar cell is used; Comparatively speaking metallurgy method has characteristics with short production cycle, that pollution is little, cost is low, is the emphasis that various countries competitively research and develop.Electron beam melting is one of important method of metallurgy method purifying polycrystalline silicon, and it can effectively reduce the foreign matter of phosphor in the polysilicon, but in the present electron beam melting purifying polycrystalline silicon process; The general direct use cold-crucible of smelting pot; Not only power loss is serious directly to use cold-crucible, and energy consumption is big, and cost is high; And cause the pollution of tramp material easily, make the purity drop of polysilicon.
Summary of the invention
The present invention overcomes above-mentioned not enough problem; The method of electron beam melting purifying polycrystalline silicon under a kind of HIGH-PURITY SILICON substrate is provided; Utilize electron beam melting at the inner one deck HIGH-PURITY SILICON substrate that forms of cold-crucible earlier, melting purifying polycrystalline silicon on this HIGH-PURITY SILICON substrate reduces energy consumption then; Avoid the pollution of crucible, effectively improve the purity of polysilicon.Another object of the present invention provides the equipment of electron beam melting purifying polycrystalline silicon under a kind of HIGH-PURITY SILICON substrate, and is simple in structure, easy to operate, and refining effect is good.
The present invention for realizing the technical scheme that above-mentioned purpose adopted is: the method for electron beam melting purifying polycrystalline silicon under a kind of HIGH-PURITY SILICON substrate, and concrete technology is:
The first step is got the raw materials ready and pre-treatment: at first in cold-crucible, fill the HIGH-PURITY SILICON material, close fire door after, extracting vacuum chamber vacuum is to 0.002Pa;
Second step formed the HIGH-PURITY SILICON substrate: unlocking electronic bundle line is that 200-500mA melts the HIGH-PURITY SILICON material fully then; Slowly reducing line is zero; Promptly in cold-crucible, form the high purity polycrystalline silicon ingot; Regulate electron beam spot and be positioned at the cold-crucible central position, after this unlocking electronic bundle line is a 150-300mA fusing high purity polycrystalline silicon ingot, forms one deck HIGH-PURITY SILICON substrate behind the 2-5min;
The 3rd step melting is purified: open feeding device at last, high phosphorus silicon material slowly falls into the molten bath continuously, and strengthen line to 300-700mA this moment; Regulate the electron beam spot position simultaneously, make the melting in the molten bath of its right side, its left side is used to melt the high phosphorus silicon material that neutralization has just fallen into the molten bath; High phosphorus silicon material fusing back forms high phosphorus silicon liquid, and high phosphorus silicon liquid melting rear impurity phosphorus obtains removing, after this among flow-guiding mouth inflow crucible; Obtain low-phosphorous silicon liquid, obtain low-phosphorous polycrystal silicon ingot after solidifying.
The said the first step is got the raw materials ready and pre-treatment: adopt mechanical pump, lobe pump and DP to the equipment extracting vacuum respectively, Vakuumkammer is extracted into below the high vacuum 0.002Pa; In water-cooled support bar, cold-crucible and water-cooled base for supporting, feed water coolant, make its temperature maintenance at 30-45 ℃; Give the electron beam gun preheating, it is 30-32kV that high pressure is set, and high pressure is closed high pressure after stablizing 5-10 minute, and it is that 100-200mA carries out preheating that the electron beam gun line is set, and after preheating 10-15 minute, closes the electron beam gun line.
Said high phosphorus silicon material is shivering material or powder.
The equipment of electron beam melting purifying polycrystalline silicon under a kind of HIGH-PURITY SILICON substrate, equipment constitutes vacuum apparatus by fire door and vacuum furnace wall, and the inner chamber of vacuum apparatus is Vakuumkammer; The water-cooled support bar is fixedly installed in vacuum furnace wall bottom left; Cold-crucible is fixedly installed on the water-cooled support bar, and the HIGH-PURITY SILICON substrate places the cold-crucible inwall, and feeding device is installed on vacuum furnace wall top left side; Electron beam gun is installed on top, vacuum furnace wall, and its lower end is over against cold-crucible; The water-cooled base for supporting is fixedly installed in vacuum furnace wall bottom, right side, and graphite block is fixedly installed on the water-cooled base for supporting, and crucible is installed on the graphite block, and the cold-crucible flow-guiding mouth is aimed at crucible.
Said vacuum is installed mechanical pump, lobe pump, DP and purging valve respectively on the furnace wall.
The present invention utilizes electron beam melting to form the high purity polycrystalline silicon substrate earlier, little line under this substrate effect then, and the polycrystalline silicon material of continuous smelting high phosphorus is removed the foreign matter of phosphor in the polysilicon fast.The high purity polycrystalline silicon substrate that forms in this method is kept apart the silicon melt and the cold-crucible of melting; Got heat insulation effect; Reduced the heat that cold-crucible is taken away, improved the temperature of melt bottom, quickened the dispensing volatile of foreign matter of phosphor and removed speed; And the HIGH-PURITY SILICON substrate has reduced, and impurity improves the purity of polysilicon to the pollution of melting polysilicon on the cold-crucible wall.This method refining effect is good, and technology is simple, and save energy reduces extraneous contamination, is fit to produce in batches.
Present device is simple in structure, and design is unique, and melting obtains the HIGH-PURITY SILICON substrate on cold-crucible, and simple to operate, cost is low, can realize continuous smelting, and production efficiency is high, is fit to large-scale industrial production.
Description of drawings
Accompanying drawing 1 is the device structure sketch of electron beam melting purifying polycrystalline silicon under a kind of HIGH-PURITY SILICON substrate.
Among the figure, 1. electron beam gun, 2. flow-guiding mouth, 3. purging valve, 4. DP; 5. lobe pump, 6. mechanical pump, 7. Vakuumkammer, 8. fire door, 9. crucible; 10. low-phosphorous silicon liquid, 11. graphite blocks, 12. water-cooled base for supporting, 13. vacuum furnace walls, 14. water-cooled support bars; 15. cold-crucible, 16. HIGH-PURITY SILICON substrates, 17. high phosphorus silicon liquid, 18. high phosphorus silicon material, 19. feeding devices.
Embodiment
Specify the present invention below in conjunction with specific embodiment and accompanying drawing, but the present invention is not limited to specific embodiment.
Embodiment 1
The equipment of electron beam melting purifying polycrystalline silicon under a kind of HIGH-PURITY SILICON substrate, equipment constitutes vacuum apparatus by fire door 8 and vacuum furnace wall 13, and the inner chamber of vacuum apparatus is Vakuumkammer 7; Water-cooled base for supporting 12 is fixedly installed in vacuum furnace wall bottom, right side, and graphite block 11 is fixedly installed on the water-cooled base for supporting, and crucible 9 is installed on the graphite block; Water-cooled support bar 14 is fixedly installed in vacuum furnace wall bottom left; Cold-crucible 15 is fixedly installed on the water-cooled support bar 14; HIGH-PURITY SILICON substrate 16 places the cold-crucible inwall, and feeding device 19 is installed on vacuum furnace wall top left side, and electron beam gun 1 is installed on top, vacuum furnace wall; Its lower end is over against cold-crucible, and mechanical pump 6, lobe pump 5, DP 4 and purging valve 3 are installed on respectively on the vacuum furnace wall 2.
Embodiment 2
Adopt embodiment 1 described equipment to carry out the method for electron beam melting purifying polycrystalline silicon under the HIGH-PURITY SILICON substrate, its concrete steps are following:
The first step is got the raw materials ready and pre-treatment: at first in cold-crucible 15, filling content of impurities is 3ppmw HIGH-PURITY SILICON material, close fire door 8 after, adopt mechanical pump 6, lobe pump 5 and 4 pairs of equipment extracting vacuum of DP respectively, Vakuumkammer 7 is extracted into high vacuum 0.0018Pa; In water-cooled support bar 14, water jacketed copper crucible 15 and water-cooled base for supporting 12, feed water coolant, make its temperature maintenance at 40 ℃; Give electron beam gun 1 preheating, it is 30kV that high pressure is set, and high pressure is closed high pressure after stablizing 5 minutes, and it is that 200mA carries out preheating that electron beam gun 1 line is set, and preheating was closed electron beam gun 1 line after 15 minutes;
Second step formed the HIGH-PURITY SILICON substrate: unlocking electronic bundle line is that 300mA melts the HIGH-PURITY SILICON material fully then; After this slowly reducing line is zero; Promptly in cold-crucible, form the high purity polycrystalline silicon ingot; Regulate electron beam spot and be located at the cold-crucible central position, after this unlocking electronic bundle line is a 200mA fusing high purity polycrystalline silicon ingot, forms one deck HIGH-PURITY SILICON substrate 16 behind the 5min;
The 3rd step melting is purified: open feeding device at last, phosphorus content is that 17ppmw high phosphorus silicon material 18 slowly falls into the molten bath continuously, and strengthen line to 400mA this moment; Regulate the electron beam spot position simultaneously; Make the melting in the molten bath of its right side, its left side is used to melt the high phosphorus silicon material 18 that neutralization has just fallen into the molten bath, and high phosphorus silicon material fusing back forms high phosphorus silicon liquid; High phosphorus silicon liquid melting rear impurity phosphorus obtains removing; After this among flowing into crucible from flow-guiding mouth, obtain low-phosphorous silicon liquid, obtain low-phosphorous polycrystal silicon ingot after solidifying.
(ICP-MS) detect, its phosphorus content is lower than 0.4ppmw, has satisfied the request for utilization of solar level silicon materials through ELAN DRC-II type inductively coupled plasma mass spectrograph equipment.
Embodiment 3
Adopt embodiment 1 described equipment to carry out the method for electron beam melting purifying polycrystalline silicon under the HIGH-PURITY SILICON substrate, its concrete steps are following:
The first step is got the raw materials ready and pre-treatment: at first in cold-crucible 15, filling content of impurities is 2ppmw HIGH-PURITY SILICON material, close fire door 8 after, adopt mechanical pump 6, lobe pump 5 and 4 pairs of equipment extracting vacuum of DP respectively, Vakuumkammer 7 is extracted into high vacuum 0.0015Pa; In water-cooled support bar 14, water jacketed copper crucible 15 and water-cooled base for supporting 12, feed water coolant, make its temperature maintenance at 40 ℃; Give electron beam gun 1 preheating, 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 1 line is set, and preheating was closed electron beam gun 1 line after 15 minutes;
Second step formed the HIGH-PURITY SILICON substrate: unlocking electronic bundle line is that 400mA melts the HIGH-PURITY SILICON material fully then; After this slowly reducing line is zero; Promptly in cold-crucible, form the high purity polycrystalline silicon ingot; Regulate electron beam spot and be located at the cold-crucible central position, after this unlocking electronic bundle line is a 300mA fusing high purity polycrystalline silicon ingot, forms one deck HIGH-PURITY SILICON substrate 16 behind the 3min;
The 3rd step melting is purified: open feeding device at last, phosphorus content is that 15ppmw high phosphorus silicon material 18 slowly falls into the molten bath continuously, and strengthen line to 500mA this moment; Regulate the electron beam spot position simultaneously; Make the melting in the molten bath of its right side, its left side is used to melt the high phosphorus silicon material 18 that neutralization has just fallen into the molten bath, and high phosphorus silicon material fusing back forms high phosphorus silicon liquid; High phosphorus silicon liquid melting rear impurity phosphorus obtains removing; After this among flowing into crucible from flow-guiding mouth, obtain low-phosphorous silicon liquid, obtain low-phosphorous polycrystal silicon ingot after solidifying.
(ICP-MS) detect, its phosphorus content is lower than 0.3ppmw, has satisfied the request for utilization of solar level silicon materials through ELAN DRC-II type inductively coupled plasma mass spectrograph equipment.
Claims (5)
1. the method for electron beam melting purifying polycrystalline silicon under the HIGH-PURITY SILICON substrate is characterized in that:
The first step is got the raw materials ready and pre-treatment: at first in cold-crucible, fill the HIGH-PURITY SILICON material, close fire door after, extracting vacuum chamber vacuum is to 0.002Pa;
Second step formed the HIGH-PURITY SILICON substrate: unlocking electronic bundle line is that 200-500mA melts the HIGH-PURITY SILICON material fully then; Slowly reducing line is zero; Promptly in cold-crucible, form the high purity polycrystalline silicon ingot; Regulate electron beam spot and be positioned at the cold-crucible central position, after this unlocking electronic bundle line is a 150-300mA fusing high purity polycrystalline silicon ingot, forms one deck HIGH-PURITY SILICON substrate behind the 2-5min;
The 3rd step melting is purified: open feeding device at last, high phosphorus silicon material slowly falls into the molten bath continuously, and strengthen line to 300-700mA this moment; Regulate the electron beam spot position simultaneously, make the melting in the molten bath of its right side, its left side is used to melt the high phosphorus silicon material that neutralization has just fallen into the molten bath; High phosphorus silicon material fusing back forms high phosphorus silicon liquid, and high phosphorus silicon liquid melting rear impurity phosphorus obtains removing, after this among flow-guiding mouth inflow crucible; Obtain low-phosphorous silicon liquid, obtain low-phosphorous polycrystal silicon ingot after solidifying.
2. the method for electron beam melting purifying polycrystalline silicon under a kind of HIGH-PURITY SILICON substrate according to claim 1; It is characterized in that: the said the first step is got the raw materials ready and pre-treatment: adopt mechanical pump, lobe pump and DP to the equipment extracting vacuum respectively, Vakuumkammer is extracted into below the high vacuum 0.002Pa; In water-cooled support bar, cold-crucible and water-cooled base for supporting, feed water coolant, make its temperature maintenance at 30-45 ℃; Give the electron beam gun preheating, it is 30-32kV that high pressure is set, and high pressure is closed high pressure after stablizing 5-10 minute, and it is that 100-200mA carries out preheating that the electron beam gun line is set, and after preheating 10-15 minute, closes the electron beam gun line.
3. the method for electron beam melting purifying polycrystalline silicon under a kind of HIGH-PURITY SILICON substrate according to claim 1 is characterized in that: said high phosphorus silicon material is shivering material or powder.
4. the equipment of electron beam melting purifying polycrystalline silicon under the HIGH-PURITY SILICON substrate, it is characterized in that: equipment constitutes vacuum apparatus by fire door (8) and vacuum furnace wall (13), and the inner chamber of vacuum apparatus is Vakuumkammer (7); Water-cooled support bar (14) is fixedly installed in vacuum furnace wall bottom left; Cold-crucible (15) is fixedly installed on the water-cooled support bar; HIGH-PURITY SILICON substrate (16) places the cold-crucible inwall; Feeding device (19) is installed on vacuum furnace wall top left side, and electron beam gun (1) is installed on top, vacuum furnace wall, and its lower end is over against cold-crucible; Water-cooled base for supporting (12) is fixedly installed in vacuum furnace wall bottom, right side, and graphite block (11) is fixedly installed on the water-cooled base for supporting, and crucible (9) is installed on the graphite block; The cold-crucible flow-guiding mouth is aimed at crucible.
5. according to the equipment of electron beam melting purifying polycrystalline silicon under the said a kind of HIGH-PURITY SILICON substrate of claim 4, it is characterized in that: mechanical pump (6), lobe pump (5), DP (4) and purging valve (3) are installed respectively on vacuum furnace wall (2).
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103818907A (en) * | 2014-03-04 | 2014-05-28 | 黄道德 | Dephosphorizing method for solar battery polycrystalline silicon |
| CN104195636A (en) * | 2014-09-01 | 2014-12-10 | 大连理工大学 | Method for rapidly preparing boron master alloy by using metallurgy method |
| CN104528732A (en) * | 2014-12-25 | 2015-04-22 | 大连理工大学 | Novel device and method for reducing energy consumption of electron beam melting technology |
| CN105129804A (en) * | 2015-09-01 | 2015-12-09 | 中国化学工程第六建设有限公司 | Production technology for polycrystalline silicon |
| CN109107492A (en) * | 2018-10-29 | 2019-01-01 | 大连颐和顺新材料科技有限公司 | A kind of the high temperature transferred arc Granulation Equipments and method of Buddha's warrior attendant wire cutting silicon powder |
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| CN102120579A (en) * | 2011-01-29 | 2011-07-13 | 大连隆田科技有限公司 | Method and device for efficiently and continuously smelting and purifying polysilicon with electron beams |
| CN102126726A (en) * | 2011-01-29 | 2011-07-20 | 大连隆田科技有限公司 | Method and equipment for efficiently purifying polysilicon powder by utilizing electron beams |
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| US20060017203A1 (en) * | 2004-06-03 | 2006-01-26 | Norichika Yamauchi | Refining apparatus for scrap silicon using an electron beam |
| CN102120579A (en) * | 2011-01-29 | 2011-07-13 | 大连隆田科技有限公司 | Method and device for efficiently and continuously smelting and purifying polysilicon with electron beams |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103818907A (en) * | 2014-03-04 | 2014-05-28 | 黄道德 | Dephosphorizing method for solar battery polycrystalline silicon |
| CN104195636A (en) * | 2014-09-01 | 2014-12-10 | 大连理工大学 | Method for rapidly preparing boron master alloy by using metallurgy method |
| CN104528732A (en) * | 2014-12-25 | 2015-04-22 | 大连理工大学 | Novel device and method for reducing energy consumption of electron beam melting technology |
| CN104528732B (en) * | 2014-12-25 | 2017-04-12 | 大连理工大学 | Novel device and method for reducing energy consumption of electron beam melting technology |
| CN105129804A (en) * | 2015-09-01 | 2015-12-09 | 中国化学工程第六建设有限公司 | Production technology for polycrystalline silicon |
| CN105129804B (en) * | 2015-09-01 | 2017-03-08 | 中国化学工程第六建设有限公司 | The production technology of polysilicon |
| CN109107492A (en) * | 2018-10-29 | 2019-01-01 | 大连颐和顺新材料科技有限公司 | A kind of the high temperature transferred arc Granulation Equipments and method of Buddha's warrior attendant wire cutting silicon powder |
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Application publication date: 20120411 |