CN202063730U - Electron beam and slag filter smelting polycrystalline silicon purifying equipment - Google Patents
Electron beam and slag filter smelting polycrystalline silicon purifying equipment Download PDFInfo
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- CN202063730U CN202063730U CN2011201554815U CN201120155481U CN202063730U CN 202063730 U CN202063730 U CN 202063730U CN 2011201554815 U CN2011201554815 U CN 2011201554815U CN 201120155481 U CN201120155481 U CN 201120155481U CN 202063730 U CN202063730 U CN 202063730U
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Abstract
The utility model belongs to the technical field of polycrystalline silicon purification by the aid of physical metallurgy, and relates to electron beam and slag filter smelting polycrystalline silicon purifying equipment. Vacuum equipment consists of a furnace door and a vacuum furnace wall, an inner cavity of the vacuum equipment is a vacuum chamber, a bar pulling mechanism is fixedly mounted at the bottom of the vacuum chamber, a smelting crucible is mounted on the bar pulling mechanism, a heating device is sleeved outside the smelting crucible, a water-cooling supporting rod is further mounted at the bottom of the vacuum chamber, a water-cooling copper crucible is mounted on the water-cooling supporting rod, a feeding device is fixedly mounted on the inner side of the top of the vacuum furnace wall above the water-cooling copper crucible, the water-cooling copper crucible is communicated with the smelting crucible via a flow guiding device, an electronic gun is mounted at the top of the vacuum furnace wall, and an air evacuation valve is mounted on the vacuum furnace wall. The electron beam and slag filter smelting polycrystalline silicon purifying equipment is simple in structure and unique in design, comprehensively utilizes electro beam smelting phosphorous removal, slag filter smelting boron removal and directional solidification metal removal techniques to removal phosphorus, boron and metal purifies in polycrystalline silicon, and is compact in structure, high in equipment integrated level, fine in purification effect and high in production efficiency.
Description
Technical field
The utility model belongs to the technical field with physical metallurgy technology purifying polycrystalline silicon, particularly a kind of equipment with the foreign matter of phosphor in the polysilicon, boron and metal removal.
Background technology
Solar grade polycrystalline silicon material is the important source material of solar cell, and 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.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 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 produces and be discontinuity, can't form in the production of Si and work continuously.
(2) 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 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.
(3) 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 by thermolysis.This method is based on chemical technology, and energy consumption is bigger, compares no clear superiority with the siemens method.
(4) 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.
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, it can effectively reduce the foreign matter of phosphor in the polysilicon, but the method for present most of electron beam melting purifying polycrystalline silicon can't effectively be removed boron impurities and metallic impurity in the polysilicon simultaneously, and two electron beam gun are all used in general electron beam melting, have the bigger shortcoming of energy consumption.Known application number is the utility model patent of 2008100713986.X, utilize electron beam melting to reach the purpose of removing phosphorus in the polysilicon, but the method that this patent is used can't effectively be removed the boron impurities in the polysilicon, need other technological process could remove boron impurities, increased process procedure, use two electron beam gun in the method that this patent is used simultaneously, energy consumption is bigger.
Summary of the invention
The utility model overcomes above-mentioned not enough problem, the equipment of a kind of electron beam and slag filter melting purifying polycrystalline silicon is provided, compact construction, comprehensive utilization electron beam melting, slag filter melting and directional solidification technique, simple to operate, purification precision height is removed phosphorus in the polysilicon, boron and metallic impurity simultaneously, reaches the service requirements of solar grade polycrystalline silicon material.
The technical scheme that the utility model is adopted for achieving the above object is: the equipment of a kind of electron beam and slag filter melting purifying polycrystalline silicon, and equipment constitutes vacuum apparatus by fire door and vacuum furnace wall, and the inner chamber of vacuum apparatus is vacuum chamber; Vacuum chamber bottom fixed installation ingot pulling mechanism, melting crucible is installed on the ingot pulling mechanism, the outer suit heating unit of melting crucible, the vacuum chamber bottom also is equipped with the water-cooled support bar, water jacketed copper crucible is installed on the water-cooled support bar, and feeding device is fixedly installed in vacuum furnace wall, water jacketed copper crucible top inside top, and water jacketed copper crucible is communicated with smelting pot by guiding device, electron beam gun is installed on top, vacuum furnace wall, and purging valve is installed on the vacuum furnace wall.
Described heating unit adopts on the base for supporting heat preservation carbon felt and graphite heater is installed from outside to inside, and base for supporting is fixedly mounted on the vacuum chamber, and ingot pulling mechanism is positioned at base for supporting; Described ingot pulling mechanism adopts water-cooled to draw graphite block is installed on the spindle blade, and smelting pot places on the graphite block.
Described guiding device adopts the spreader plate that has material falling hole to place on the graphite bracing frame, and the diversion trench two ends are overlapped in spreader plate and water jacketed copper crucible edge respectively, and the graphite bracing frame is installed on heat preservation carbon felt and the graphite heater.
Described spreader plate edge height, middle low, middle uniform distribution material falling hole; Spreader plate adopts fusing point to be higher than silicon, and hot strength is big, makes greater than 90 ° material with the silicon wetting angle, as quartzy or ceramic.
The utility model device structure is simple, design is unique, an equipment complex utilizes the electron beam melting dephosphorization, slag filter melting removes boron and directional freeze and removes the technology of metal and remove phosphorus in the polysilicon, boron and metallic impurity, compact construction, the device integration height, reduced process procedure, melted silicon after phosphorus removed fuses among the slag former liquation continuously uniformly, and contact area increases between silicon and the slag agent, the temperature of reaction raising, and graphite heating body is for the not influence of emission of electron beam, help improving the speed and the degree of reaction, refining effect is good, the production efficiency height, save energy is fit to large-scale industrial production.
Description of drawings
Accompanying drawing 1 is the device structure sketch of a kind of electron beam and slag filter melting purifying polycrystalline silicon.
Among the figure, 1. electron beam gun, 2. diversion trench, 3. purging valve, 4. diffusion pump, 5. lobe pump, 6. mechanical pump, 7. vacuum chamber, 8. fire door, 9. spreader plate, 10. graphite bracing frame, 11. heat preservation carbon felts, 12. graphite heater, 13. the slag former liquation, 14. smelting pots, 15. graphite blocks, 16. base for supporting, 17. water-cooled is drawn spindle blade, 18. vacuum furnace walls, 19. water-cooled support bars, 20. water jacketed copper crucible, 21. melted silicon, 22. high phosphorus, high boron, high metal polycrystalline silicon material, 23. feeding devices.
Embodiment
Describe the utility model in detail below in conjunction with specific embodiment and accompanying drawing, but the utility model is not limited to specific embodiment.
Embodiment 1
The equipment of a kind of electron beam and slag filter melting purifying polycrystalline silicon, equipment constitutes vacuum apparatus by fire door 8 and vacuum furnace wall 2, and the inner chamber of vacuum apparatus is vacuum chamber 7; Right side, vacuum chamber 7 bottom fixed installation base for supporting 16, on the vacuum furnace wall 2 in the base for supporting 16 water-cooled is installed and draws spindle blade 17, graphite block 15 is installed in water-cooled and draws on the spindle blade 17, smelting pot 14 places on the graphite block 15, heat preservation carbon felt 11 and graphite heater 12 are installed on the base for supporting 16 from outside to inside, and guiding device is installed on heat preservation carbon felt 11 and the graphite heater 12; Vacuum chamber 7 bottom left are equipped with water-cooled support bar 19, water jacketed copper crucible 20 is installed on the water-cooled support bar 19, feeding device 23 is fixedly installed in 2 inside top positions, vacuum furnace wall, water jacketed copper crucible 20 top, guiding device is used to connect water jacketed copper crucible 20 and smelting pot 14, electron beam gun 1 is installed on 2 tops, vacuum furnace wall, and purging valve 3 is installed on the vacuum furnace wall 2; Guiding device adopts graphite bracing frame 10 to be installed on heat preservation carbon felt 11 and the graphite heater 12, and spreader plate 9 places on the graphite bracing frame 10, and diversion trench 2 two ends are overlapped in spreader plate 9 and water jacketed copper crucible 20 edges respectively; Spreader plate 9 edge height, middle low, the centre has material falling hole, and spreader plate 9 adopts fusing points to be higher than silicon, and hot strength is big, makes greater than 90 ° material such as quartz or pottery with the silicon wetting angle.
Embodiment 2
Adopt embodiment 1 described equipment to carry out the method for electron beam and slag filter melting purifying polycrystalline silicon, its concrete steps are as follows:
The first step is got the raw materials ready: with mass percent is SiO
270%, CaO20% and Na
2CO
310% slag former 1200g slag former is tiled in smelting pot 14 bottoms, and this moment, the add-on of slag former was to be advisable in 1/6 position of smelting pot 14 volumes, closed fire door 8;
The second step pre-treatment: adopt mechanical pump 6, lobe pump 5 that vacuum chamber 7 is extracted into rough vacuum 7Pa respectively, with diffusion pump 4 vacuum chamber 7 is extracted into high vacuum 0.0015Pa again; Draw in the spindle blade 17 to water-cooled support bar 19, water jacketed copper crucible 20 and water-cooled to 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 10 minutes;
Molten dissolving agent of the 3rd step and dephosphorization: give graphite heater 12 energisings, by graphite heating the slag former fusing is formed slag former liquation 13, and keep liquid state; Simultaneously by feeding device 23 add continuously in water jacketed copper crucible 20 that phosphorus content is 0.0022%, boron content is 0.0018%, the metallic impurity total content is 0.035% polycrystalline silicon material 22, open the high pressure and the line of electron beam gun 1, after stable, by the polycrystalline silicon material 22 of electron beam gun 1 with high phosphorus, high boron and high metal in the line bombardment water jacketed copper crucible 20 of 300mA, make its fusing form melted silicon 21, the foreign matter of phosphor in the electron beam melting process in the melted silicon obtains removing the low-phosphorous melted silicon of formation;
The 4th step removed boron and removes metal: low-phosphorous melted silicon enters guiding device by the flow-guiding mouth on the water jacketed copper crucible 20, under the guiding device guiding, low-phosphorous melted silicon is continuous, evenly, dispersive fuses among the slag former liquation 13, strengthen graphite heater 12 power, make melt temperature reach 1450 ℃, in the process of fusing into, boron impurities and slag former in the melted silicon react, boron impurities obtains removing, melted silicon after boron impurities is removed constantly sinks, assemble in smelting pot 14 bottoms, when treating that liquation in the melting crucible 14 is filled, stop to add polycrystalline silicon material, close electron beam gun 1 after 10 minutes, and the liquation in the smelting pot 14 heating kept liquid reaction 10 minutes, draw spindle blade 17 to pull down ingot by water-cooled at last, liquation begins directional solidification growth, metallic impurity and waste residue are constantly assembled to the silicon ingot top, after solidifying fully and reducing to room temperature, open purging valve 19 venting, take out silicon ingot, cut the higher silico briquette of silicon ingot top waste residue and metal content, can obtain phosphorus, the polycrystal silicon ingot that boron and metals content impurity are lower.Through ELAN DRC-II type inductively coupled plasma mass spectrograph equipment (ICP-MS) detect, the content of phosphorus impurities is reduced to below 0.00004%, the content of boron impurity is reduced to below 0.00008%, the metallic impurity total content is reduced to below 0.00015%, has reached the service requirements of solar level silicon materials.
Claims (5)
1. the equipment of electron beam and slag filter melting purifying polycrystalline silicon, it is characterized in that: equipment constitutes vacuum apparatus by fire door (8) and vacuum furnace wall (2), and the inner chamber of vacuum apparatus is vacuum chamber (7); Vacuum chamber (7) bottom fixed installation ingot pulling mechanism, melting crucible is installed on the ingot pulling mechanism, the outer suit heating unit of melting crucible, vacuum chamber (7) bottom also is equipped with water-cooled support bar (19), water jacketed copper crucible (20) is installed on the water-cooled support bar (19), feeding device (23) is fixedly installed in vacuum furnace wall (2), water jacketed copper crucible (20) top inside top, water jacketed copper crucible (20) is communicated with smelting pot (14) by guiding device, electron beam gun (1) is installed on top, vacuum furnace wall (2), and purging valve (3) is installed on the vacuum furnace wall (2).
2. the equipment of a kind of electron beam according to claim 1 and slag filter melting purifying polycrystalline silicon, it is characterized in that: described heating unit adopts on the base for supporting (16) heat preservation carbon felt (11) and graphite heater (12) is installed from outside to inside, base for supporting (16) is fixedly mounted on the vacuum chamber, ingot pulling mechanism is positioned at base for supporting; Described ingot pulling mechanism adopts water-cooled to draw spindle blade (17) to go up graphite block (15) is installed, and smelting pot (14) places on the graphite block (15).
3. the equipment of a kind of electron beam according to claim 1 and slag filter melting purifying polycrystalline silicon, it is characterized in that: described guiding device adopts the spreader plate (9) that has material falling hole to place on the graphite bracing frame (10), diversion trench (2) two ends are overlapped in spreader plate (9) and water jacketed copper crucible (20) edge respectively, and graphite bracing frame (10) is installed on heat preservation carbon felt (11) and the graphite heater (12).
4. the equipment of a kind of electron beam according to claim 3 and slag filter melting purifying polycrystalline silicon is characterized in that: described spreader plate (9) edge height, and middle low, middle uniform distribution material falling hole.
5. the equipment of a kind of electron beam according to claim 3 and slag filter melting purifying polycrystalline silicon, it is characterized in that: described spreader plate (9) adopts fusing point to be higher than silicon, and hot strength is big, makes greater than 90 ° material with the silicon wetting angle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011201554815U CN202063730U (en) | 2011-05-16 | 2011-05-16 | Electron beam and slag filter smelting polycrystalline silicon purifying equipment |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011201554815U CN202063730U (en) | 2011-05-16 | 2011-05-16 | Electron beam and slag filter smelting polycrystalline silicon purifying equipment |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102145894A (en) * | 2011-05-16 | 2011-08-10 | 大连隆田科技有限公司 | Method and device for smelting and purifying polysilicon by using electron beams and adopting slag filtering |
| CN103086379A (en) * | 2013-01-23 | 2013-05-08 | 大连理工大学 | Radiation-intercepting device of crucible for electron-beam smelting |
| CN103435043A (en) * | 2013-08-28 | 2013-12-11 | 青岛隆盛晶硅科技有限公司 | Device and process method for preparing polycrystalline silicon through coupling of electron beam smelting and crystal growing technology |
| TWI580919B (en) * | 2015-10-14 | 2017-05-01 | 國立清華大學 | Composite structures of multi-crucibles and their high-temperature adiabatic heating method in vacuum arc melting process |
-
2011
- 2011-05-16 CN CN2011201554815U patent/CN202063730U/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102145894A (en) * | 2011-05-16 | 2011-08-10 | 大连隆田科技有限公司 | Method and device for smelting and purifying polysilicon by using electron beams and adopting slag filtering |
| CN103086379A (en) * | 2013-01-23 | 2013-05-08 | 大连理工大学 | Radiation-intercepting device of crucible for electron-beam smelting |
| CN103086379B (en) * | 2013-01-23 | 2014-12-10 | 大连理工大学 | Radiation-intercepting device of crucible for electron-beam smelting |
| CN103435043A (en) * | 2013-08-28 | 2013-12-11 | 青岛隆盛晶硅科技有限公司 | Device and process method for preparing polycrystalline silicon through coupling of electron beam smelting and crystal growing technology |
| CN103435043B (en) * | 2013-08-28 | 2015-05-27 | 青岛隆盛晶硅科技有限公司 | Device and process method for preparing polycrystalline silicon through coupling of electron beam smelting and crystal growing technology |
| TWI580919B (en) * | 2015-10-14 | 2017-05-01 | 國立清華大學 | Composite structures of multi-crucibles and their high-temperature adiabatic heating method in vacuum arc melting process |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| ASS | Succession or assignment of patent right |
Owner name: QINGDAO LONGSHENG CRYSTAL SILICONE TECHNOLOGY CO., Free format text: FORMER OWNER: DALIAN LONGTIAN TECH. CO., LTD. Effective date: 20120424 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| COR | Change of bibliographic data |
Free format text: CORRECT: ADDRESS; FROM: 116025 DALIAN, LIAONING PROVINCE TO: 266000 QINGDAO, SHANDONG PROVINCE |
|
| TR01 | Transfer of patent right |
Effective date of registration: 20120424 Address after: Pudong solar energy industry base in Jimo city of Shandong Province, Qingdao City, 266000 Patentee after: Qingdao Longsheng Crystalline Silicon Science & Technology Co., Ltd. Address before: High tech Industrial District of Dalian City, Liaoning province 116025 Lixian Street No. 32 B block 508 Patentee before: Dalian Longtian Tech. Co., Ltd. |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20160504 Address after: 116025 Liaoning city of Dalian province high tech Industrial Park, Lixian Street No. 32 block B room 508-2 Patentee after: Dalian Longsheng Technology Co., Ltd. Address before: Pudong solar energy industry base in Jimo city of Shandong Province, Qingdao City, 266000 Patentee before: Qingdao Longsheng Crystalline Silicon Science & Technology Co., Ltd. |
|
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20111207 Termination date: 20190516 |