CN202046890U - Device for purifying polysilicon through vacuum melting of shallow molten pool - Google Patents
Device for purifying polysilicon through vacuum melting of shallow molten pool Download PDFInfo
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- CN202046890U CN202046890U CN201120155482XU CN201120155482U CN202046890U CN 202046890 U CN202046890 U CN 202046890U CN 201120155482X U CN201120155482X U CN 201120155482XU CN 201120155482 U CN201120155482 U CN 201120155482U CN 202046890 U CN202046890 U CN 202046890U
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Abstract
The utility model belongs to the technical field of purifying polysilicon with a physical metallurgy technology, and provides a device for purifying the polysilicon through vacuum melting of a shallow molten pool, a vacuum device consists of a furnace cover and a vacuum furnace wall, an inner cavity of the vacuum device is a vacuum chamber, an ingot pulling mechanism is arranged at the bottom of the vacuum chamber, a melting crucible is arranged on the ingot pulling mechanism, a heating device is arranged outside the melting crucible, an electric lifting device is arranged on an outer wall of the top of the vacuum chamber, the electric lifting device is in driving connection with the upper end of a lifting pull rod, the lower end of the lifting pull rod is connected onto a suspension clamping device in the vacuum chamber by penetrating through a vacuum furnace wall, and the suspension clamping device is above the melting crucible. The utility model has a compact structure and a unique design, integrates a high-temperature and high-vacuum large-area shallow molten pool melting technology with a directional solidification technology to remove phosphorus and metal impurities in the polysilicon, improves a production efficiency, has an excellent removal effect, and integrates dual effects of removing phosphorus and removing metal, thus, the utility model is suitable for a large-scale industrial production.
Description
Technical field
The utility model belongs to the technical field with physical metallurgy technology purifying polycrystalline silicon, particularly a kind of equipment with phosphorus in the polysilicon and metallic impurity 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 present 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.As known application number is the patent of invention of 2008100713986.X, utilizes the electron beam melting of bielectron rifle to remove foreign matter of phosphor and metal, but uses the bielectron rifle in this method, and energy consumption is bigger, and the surface-area in molten bath is little in the water jacketed copper crucible, and the speed of removing phosphorus is slower.
Summary of the invention
The utility model overcomes above-mentioned not enough problem, a kind of equipment of shallow pool vacuum melting purifying polycrystalline silicon is provided, compact construction, high surface area shallow pool melting polysilicon and directional solidification technique under comprehensive utilization high temperature, the high vacuum, easy handling, the function practicality, controllability is stronger, rapid evaporation is removed foreign matter of phosphor and the directed metallic impurity of removing, and 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: a kind of equipment of shallow pool vacuum melting purifying polycrystalline silicon, equipment constitutes vacuum apparatus by bell and vacuum furnace wall, the inner chamber of vacuum apparatus is vacuum chamber, the vacuum chamber bottom is equipped with ingot pulling mechanism, melting crucible is installed on the ingot pulling mechanism, melting crucible is equipped with heating unit outward, the lifting electric device is installed on the vacuum chamber top exterior walls, the lifting electric device drives and connects the lifter drawing bar upper end, the lifter drawing bar lower end is passed the vacuum furnace wall and is connected on the interior suspension gripping unit of vacuum chamber, hangs gripping unit and is positioned at the melting crucible top.
Described suspension gripping unit is by fixer, rotation axis, binding clasp, fishbolt constitutes, and fixer is loaded on the lifter drawing bar bottom, and fixer two ends symmetric position is equipped with two rotation axiss, a binding clasp is installed on each rotation axis, is connected by fishbolt between fixer and the binding clasp; Hang gripping unit and be installed on the lifter drawing bar bottom, can fix or rotate around lifter drawing bar; Between described lifter drawing bar and the vacuum furnace wall sealing-ring being installed seals.
Described suspension gripping unit can clamp circle, square or erose silicon rod.
Described ingot pulling mechanism adopts graphite block to be installed on water-cooled and draws on the spindle blade, and smelting pot is installed on the graphite block.
Described heating unit is made of ruhmkorff coil, graphite sleeve and heat preservation carbon felt, and ruhmkorff coil, graphite sleeve and heat preservation carbon felt are installed on the base for supporting from outside to inside, and base for supporting is fixedly mounted on outside the ingot pulling mechanism of vacuum chamber bottom.
The utility model compact equipment, design is unique, and the technology of integral high temperature, the shallow pool melting of high vacuum big area and directional freeze is removed foreign matter of phosphor and the metal in the polysilicon.The polycrystalline silicon rod of high phosphorus is hung on the top of HIGH-PURITY SILICON liquation by the suspension gripping unit, after the fusing of HIGH-PURITY SILICON liquation, polycrystalline silicon rod begins slow decline, the silicon rod surface temperature raises after entering induction region, silicon rod is preheated, when silicon rod with begin fusing after the HIGH-PURITY SILICON molten bath contacts, and spread out rapidly in weld pool surface formation shallow-layer molten bath, because the phosphorus saturated vapor pressure in the silicon is bigger, at high temperature, easily evaporation and remove the high temperature of this moment of weld pool surface under the high vacuum, the large-area shallow-layer of high vacuum molten bath provides very favorable condition for the removal of phosphorus, and foreign matter of phosphor will be fast, effectively evaporation, thereby being evacuated device takes away, after this directional freeze is removed metallic impurity, has improved production efficiency, and removal effect is good, integrated dephosphorization and remove the double effects of metal is fit to large-scale industrial production.
Description of drawings
Accompanying drawing 1 is a kind of device structure sketch of shallow pool vacuum melting purifying polycrystalline silicon.Among the figure, 1. lifting electric device, 2. lifter drawing bar, 3. vacuum chamber, 4. bell, 5. fixer, 6. rotation axis, 7. binding clasp, 8. fishbolt, 9. high phosphorus, high metal silicon rod, 10. heat preservation carbon felt, 11. graphite sleeves, 12. ruhmkorff coil, 13. smelting pots, 14. HIGH-PURITY SILICON liquations, 15. graphite blocks, 16. base for supporting, 17. water-cooleds are drawn spindle blade, 18. vacuum furnace walls, 19. purging valves, 20. mechanical pump, 21. lobe pumps, 22. diffusion pump.
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 shallow pool vacuum melting purifying polycrystalline silicon as shown in Figure 1, its equipment constitutes vacuum apparatus by bell 4 and vacuum furnace wall 18, and the inner chamber of vacuum apparatus is vacuum chamber 3.Vacuum chamber 3 bottoms fixed installation base for supporting 16, ruhmkorff coil 12, graphite sleeve 11 and heat preservation carbon felt 10 are installed on the base for supporting 16 from outside to inside, graphite sleeve 11 is used for heating to the silicon material in early days and under the nonconducting situation of silicon material of induction heating, heat preservation carbon felt 10 is used for the directional freeze process and prevents that heat scatters and disappears from sidewall, vacuum chamber bottom in the base for supporting 16 is equipped with water-cooled and draws spindle blade 17, graphite block 15 is installed on water-cooled and draws on the spindle blade 17, and smelting pot 13 is installed on the graphite block 15.
On vacuum chamber 3 top exterior walls lifting electric device 1 is installed, lifter drawing bar 2 upper ends link to each other with lifting electric device 1, the lifter drawing bar lower end is passed vacuum furnace wall 18 and is connected on the interior suspension gripping unit of vacuum chamber, lifting electric device 1 can drive lifter drawing bar 2 and move up and down, its movement velocity can be regulated, and speed is between 10mm/min-200mm/min.
Hang gripping unit and be installed on lifter drawing bar 2 bottoms, and can be that rotate in the axle center, also can maintain static with lifter drawing bar 2; Hang gripping unit by fixer 5, rotation axis 6, binding clasp 7, fishbolt 8 constitutes, fixer 5 is loaded on lifter drawing bar 2 bottoms, fixer 5 two ends symmetric positions are equipped with two rotation axiss 6, a binding clasp 7 is installed on each rotation axis, is connected by fishbolt 8 between fixer and the binding clasp; Hang gripping unit and can clamp circle, square or erose silicon rod, in the time of the dress silicon rod, suspension is stepped up device rise to the limes superiors position, open fishbolt 8, binding clasp and fixer are opened certain space, silicon rod is easily clamped one to be stretched among this space, fishbolt is connected between binding clasp and the fixer, screws to fix behind the bolt and hang silicon rod, hang the silicon ingot quality as design in this example and be 20kg to the maximum.
Between lifter drawing bar and the vacuum furnace wall sealing-ring is installed and seals, thereby guarantee that lifter drawing bar can not leak gas in the rise and fall process and between the furnace wall, thereby guarantee that vacuum tightness can not change.
Embodiment 2
Adopt embodiment 1 described equipment to carry out shallow pool vacuum melting purifying polycrystalline silicon, its concrete steps are as follows:
The first step is got the raw materials ready: fall pull bar 2 by promoting on the lifting electric device 1, lifter drawing bar 2 drives the suspension gripping unit and rises to the limes superiors position, adding 500g content of impurities is 0.0002% high purity polycrystalline silicon material in smelting pot 13, the foreign matter of phosphor content that then 4 quality is 1000g is respectively 0.0012%, 0.0015%, 0.0010%, 0.0013%, the metallic impurity total content is respectively 0.013%, 0.011%, 0.017%, 0.019%, and the polysilicon pole of quality is clamped in and hangs on the gripping unit;
The second step pre-treatment: after closing bell 4, adopt mechanical pump 20, lobe pump 21 and 22 pairs of equipment extracting vacuum of diffusion pump respectively, vacuum chamber 3 is extracted into high vacuum 0.0009Pa; Draw in the spindle blade 17 to water-cooled to feed water coolant, make its temperature maintenance at 40 ℃;
The 3rd step melted silicon material: give ruhmkorff coil 12 energisings, under 1440 ℃ condition, melt high purity polycrystalline silicon material in the smelting pot 13 by induction heating, form the HIGH-PURITY SILICON liquation, and keep liquid state, the fusing back increases the power of ruhmkorff coil 12 fully, makes the melted silicon temperature reach 1600 ℃;
The 4th step purified: drive lifter drawing bar 2 suspension gripping units by lifting electric device 1 and move downward, the feasible high phosphorus that hangs on HIGH-PURITY SILICON liquation 14 tops, high metal silicon rod 9 with the speed of 20mm/min downward vertically, extend among the melted silicon slowly, high phosphorus, high Pure Silicon Metal nose constantly melts the formation high phosphorus, the shallow-layer molten bath of high metal, foreign matter of phosphor constantly evaporates in the shallow-layer molten bath and obtains removing, treat high phosphorus at last, after high metal silicon rod fuses into the molten bath fully, induction heating makes in the smelting pot 13 and liquidly to keep 10min under 1500 ℃ of temperature, draw spindle blade 17 to pull down ingot by water-cooled, carry out directional freeze, metallic impurity are assembled to the liquation top, all solidify up to liquid state, stop to draw ingot and stop to ruhmkorff coil 12 energising, continue to vacuumize 30min, open purging valve 19 venting, open bell 4, take out silicon ingot, cut the higher polysilicon of silicon ingot top metal foreign matter content, can obtain the lower polycrystal silicon ingot of phosphorus and metals content impurity.(ICP-MS) detects, and the content of boron is reduced to below 0.0001%, and the metallic impurity total content is reduced to below 0.00018%, has reached the service requirements of solar level silicon materials through ELAN DRC-II type inductively coupled plasma mass spectrograph equipment.
Claims (7)
1. the equipment of a shallow pool vacuum melting purifying polycrystalline silicon, it is characterized in that: equipment constitutes vacuum apparatus by bell and vacuum furnace wall, the inner chamber of vacuum apparatus is vacuum chamber, the vacuum chamber bottom is equipped with ingot pulling mechanism, melting crucible is installed on the ingot pulling mechanism, melting crucible is equipped with heating unit outward, the lifting electric device is installed on the vacuum chamber top exterior walls, the lifting electric device drives and connects the lifter drawing bar upper end, the lifter drawing bar lower end is passed the vacuum furnace wall and is connected on the interior suspension gripping unit of vacuum chamber, hangs gripping unit and is positioned at the melting crucible top.
2. the equipment of a kind of shallow pool vacuum melting purifying polycrystalline silicon according to claim 1, it is characterized in that: described suspension gripping unit is by fixer, rotation axis, binding clasp, fishbolt constitutes, fixer is loaded on the lifter drawing bar bottom, fixer two ends symmetric position is equipped with two rotation axiss, a binding clasp is installed on each rotation axis, is connected by fishbolt between fixer and the binding clasp.
3. the equipment of a kind of shallow pool vacuum melting purifying polycrystalline silicon according to claim 1 is characterized in that: described suspension gripping unit is installed on the lifter drawing bar bottom, can fix or rotates around lifter drawing bar.
4. the equipment of a kind of shallow pool vacuum melting purifying polycrystalline silicon according to claim 1 is characterized in that: between described lifter drawing bar and the vacuum furnace wall sealing-ring is installed and seals.
5. the equipment of a kind of shallow pool vacuum melting purifying polycrystalline silicon according to claim 1 is characterized in that: described suspension gripping unit can clamp circle, square or erose silicon rod.
6. the equipment of a kind of shallow pool vacuum melting purifying polycrystalline silicon according to claim 1 is characterized in that: described ingot pulling mechanism adopts graphite block to be installed on water-cooled and draws on the spindle blade, and smelting pot is installed on the graphite block.
7. the equipment of a kind of shallow pool vacuum melting purifying polycrystalline silicon according to claim 1, it is characterized in that: described heating unit is made of ruhmkorff coil, graphite sleeve and heat preservation carbon felt, ruhmkorff coil, graphite sleeve and heat preservation carbon felt are installed on the base for supporting from outside to inside, and base for supporting is fixedly mounted on outside the ingot pulling mechanism of vacuum chamber bottom.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201120155482XU CN202046890U (en) | 2011-05-16 | 2011-05-16 | Device for purifying polysilicon through vacuum melting of shallow molten pool |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201120155482XU CN202046890U (en) | 2011-05-16 | 2011-05-16 | Device for purifying polysilicon through vacuum melting of shallow molten pool |
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| CN202046890U true CN202046890U (en) | 2011-11-23 |
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| CN201120155482XU Expired - Fee Related CN202046890U (en) | 2011-05-16 | 2011-05-16 | Device for purifying polysilicon through vacuum melting of shallow molten pool |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102145895A (en) * | 2011-05-16 | 2011-08-10 | 大连隆田科技有限公司 | Method and equipment for purifying polysilicon by utilizing shallow molten pool to carry out vacuum smelting |
-
2011
- 2011-05-16 CN CN201120155482XU patent/CN202046890U/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102145895A (en) * | 2011-05-16 | 2011-08-10 | 大连隆田科技有限公司 | Method and equipment for purifying polysilicon by utilizing shallow molten pool to carry out vacuum smelting |
| CN102145895B (en) * | 2011-05-16 | 2012-10-03 | 大连隆田科技有限公司 | Method and equipment for purifying polysilicon by utilizing shallow molten pool to carry out vacuum smelting |
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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: DALIAN LONGSHENG TECHNOLOGY CO., LTD. Free format text: FORMER OWNER: DALIAN LONGTIAN TECH. CO., LTD. Effective date: 20130802 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20130802 Address after: Dalian high tech park, 116025 Liaoning province Lixian Street No. 32 B-508-2 Patentee after: Dalian Longsheng 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. |
|
| ASS | Succession or assignment of patent right |
Owner name: GAOYOU INSTITUTE OF DALIAN UNIVERSITY OF TECHNOLOG Free format text: FORMER OWNER: DALIAN LONGSHENG TECHNOLOGY CO., LTD. Effective date: 20131205 |
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| 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: 225600 YANGZHOU, JIANGSU PROVINCE |
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| TR01 | Transfer of patent right |
Effective date of registration: 20131205 Address after: 225600, No. 1, outer ring road, Chengnan Economic Zone, Gaoyou, Jiangsu, Yangzhou Patentee after: Gaoyou Institute of Dalian University of Technology Co., Ltd. Address before: Dalian high tech park, 116025 Liaoning province Lixian Street No. 32 B-508-2 Patentee before: Dalian Longsheng Technology Co., Ltd. |
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| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20111123 Termination date: 20150516 |
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| EXPY | Termination of patent right or utility model |