CN102259867A - Energy saving device for directional solidification and impurity removal of metallurgical silicon - Google Patents
Energy saving device for directional solidification and impurity removal of metallurgical silicon Download PDFInfo
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- CN102259867A CN102259867A CN 201110152836 CN201110152836A CN102259867A CN 102259867 A CN102259867 A CN 102259867A CN 201110152836 CN201110152836 CN 201110152836 CN 201110152836 A CN201110152836 A CN 201110152836A CN 102259867 A CN102259867 A CN 102259867A
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Abstract
The invention relates to an energy saving device for the directional solidification and impurity removal of metallurgical silicon. The device is a rectangular body and comprises an upper heat preservation cover, a middle heat preservation sleeve, a lower bottom plate rail frame, a composite die, a heat conducting plate and a water-cooled copper disc, wherein the water-cooled copper disc is arranged in the middle of the lower bottom plate rail frame; the heat conducting plate is arranged on the upper part of the water-cooled copper disc; the composite die is arranged on the upper part of the heat conducting plate; the periphery of the composite die is filled with silicon carbide particles with supporting and heat preservation effects; and a sealing ring is arranged between the upper heat preservation cover and the middle heat preservation sleeve. The device is suitable for the directional solidification and non-vacuum production of the metallurgical silicon by a casting method, has low manufacturing cost and energy consumption and small maintenance amount, is conveniently and safely used, and is environment-friendly, directional solidification and purification effects are achieved by a simple device, product quality is improved, and production cost is reduced.
Description
Technical field
The invention belongs to metallurgy method purifying polycrystalline silicon technical field, especially relate to a kind of energy saver that is used for the removal of impurities of metalluragical silicon directional freeze.
Background technology
In order further to improve the quality of metalluragical silicon, each enterprise all takes various way measure both at home and abroad, and for example: raw material, stove blow chlorine, oxygen blast refining outward, add solvent, directional freeze etc. according to qualifications, are obtaining good effect aspect the various impurity of removal.Wherein directional solidification processes is the important step that metallurgy method prepares solar-grade polysilicon, it is to change by the controlled temperature field to make the silicon ingot unidirectional growth, utilize the effect of segregation major metal impurity element Fe, Al, Ca, Ti, Cu, Zn, Mn etc. that segregation coefficient is little to gather the silicon ingot solidification end, by intercepting the many parts of terminal impurity, obtain silicon through purifying.
At present, polycrystalline silicon ingot or purifying furnace is the fairly perfect equipment of silicon materials directional freeze performance, this equipment judges automatically that by pumped vacuum systems, heating system, temp measuring system, thermal insulation layer jacking system, pressure control system and melting crystal system, trouble diagnosis warning, powerful computer control system etc. form, be used for solar energy polycrystal silion cell section silicon ingot ingot casting more, also be useful on the use of purifying once more of the higher polycrystalline silicon material of quality.Patent of invention CN85100519 " polysilicon ingot process that the battery used of a kind of orientational solidification and growth for solar battery is used ", CN101323972 " a kind of polysilicon directional freezing equipment ", CN101898763 " a kind of directional freeze preparation method of polycrystalline silicon ", CN85100529 " polysilicon ingot process that a kind of orientational solidification and growth for solar battery is used " etc., these disclosed patent applications also all are the inventions at solar cell polysilicon casting ingot process and equipment of similar polycrystalline silicon ingot or purifying furnace, because this kind equipment all needs vacuum system, heating system, temp measuring system etc., need be with silicon materials remelting in equipment, so it is higher that its equipment has cost, production cycle is long, and monomer solidifies shortcomings such as power consumption is big.The quality of metalluragical silicon (2N level) is than polysilicon (5～6N) low 3～4 orders of magnitude, foreign matter content is many, as direct use polycrystalline silicon ingot or purifying furnace directional freeze, can cause that the rapid ageing of ingot furnace graphite piece, the serious crystallization of quartz ceramic crucible cause Lou silicon accident etc., polycrystalline silicon ingot or purifying furnace expensive is not suitable for the requirement of metalluragical silicon directional freeze.
Summary of the invention
The objective of the invention is at existing technological difficulties problem in the present existing metalluragical silicon directional freeze; a kind of energy saver that is used for the removal of impurities of metalluragical silicon directional freeze is provided; this installs, and single stove production capacity is big, simple for process, the production run cost is low, refining effect good, is suitable for large-scale production.
To achieve these goals, technical solution of the present invention is:
The energy saver of metalluragical silicon directional freeze removal of impurities, the directional freeze principle that adopts teeming practice and heat-exchanging method (HME) to combine, device is cuboid, this device comprises that insulation cover, middle muff, lower shoe rail car are configured to, composite die, heat-conducting plate and water-cooled copper dish, the water-cooled copper dish is located at the centre of lower shoe track vehicle frame, heat-conducting plate is located at the top of water-cooled copper dish, composite die is arranged at the top of heat-conducting plate, filled the silicon-carbide particle of support and insulation effect around the composite die, between last insulation cover and the middle muff sealing-ring has been arranged.Last insulation cover comprises suspension ring, steel bonnet, polycrystalline ceramic fiber layer, crystal whisker of hexa potassium titanate layer, corundum top board, outermost layer is the steel bonnet, innermost layer is equipped with the corundum top board, and middle polycrystalline ceramic fiber layer and the crystal whisker of hexa potassium titanate layer settled is equipped with suspension ring on the top board of steel bonnet.
Middle muff comprises steel boiler clothing, polycrystalline ceramic fiber layer, crystal whisker of hexa potassium titanate layer, corundum side plate, and outermost layer is the steel boiler clothing, and innermost layer is equipped with the corundum side plate, middle polycrystalline ceramic fiber layer and the crystal whisker of hexa potassium titanate layer settled.
The lower shoe rail car is set up and is equipped with 4 rail wheels, and rail wheel is installed on the steel substrate, and the water-cooled copper dish is placed in the centre of lower shoe track vehicle frame.
Composite die comprises graphite base plate and corundum riser, and places the top of heat-conducting plate, has filled the silicon-carbide particle of support and insulation effect all around, and this particle sub-circular, granularity are the 4-8 millimeter.The middle part of heat-conducting plate and water-cooled copper dish is equipped with thermopair.Surface-coated one deck silicon nitride releasing agent of composite die.
The present invention has the following advantages:
1, after the employing technique scheme, the present invention all adopts crystal whisker of hexa potassium titanate and corundum plate to make lagging material because of top and side all around, make that thermosteresis is few in the device, heat storage capacity is strong, hard carbon fibrefelt than present ingot furnace has more the insulation advantage, need not to carry out again boosting to keep the silicon ingot upper temp, temperature when only needing silicon liquid to pour into gets final product greater than 1600 ℃, is rationally utilizing aspect the heat energy advantage remarkable; Simultaneously, also satisfy the processing requirement of in atmospheric environment, using, broken away from the constraint of directional freeze in vacuum and protection of inert gas environment.
2, composite die of the present invention adopts integrated mode; internal surface applies one deck silicon nitride releasing agent; promptly be convenient to the silicon ingot demoulding; protected mould again; sidepiece filling silicon-carbide particle makes mould in conjunction with firm, tight around this outer mold; silicon liquid can seepage, improve effectively mould the repeated use number of times, reduce the subsidiary material consumption, tangible economic benefit is arranged.
3, the every stove of the present invention can carry out the directional freeze purification to the metalluragical silicon that reaches 1000Kg, and every stove treatment time is 48～72 hours, the silicon ingot pore-free after the directional freeze, flawless.
4, unusual effect of the present invention is that the radiating mode of device interior liquid metalluragical silicon is effectively controlled, form one and have only the bottom heat radiation, and the top reaches side adiabatic thermal field system all around, the top and the side direction of thermal field do not have thermograde, the control of the cooling water flow by bottom water-cooled copper dish, make silicon liquid that certain thermograde be arranged up and down, heat only dispels the heat along the bottom single direction, reaching the silicon liquid temp progressively descends from bottom to top, the slow crystallization and freezing of molten silicon liquid, keep the level all the time of solid-liquid interface to rise simultaneously, obtain good directional solidification effect, to remove the low impurity element of segregation coefficient in the metalluragical silicon.
5, the present invention is applicable to teeming practice metalluragical silicon directional freeze, antivacuum production, equipment manufacturing cost is low, energy consumption is low, maintenance capacity is little and convenient, safe in utilization, non-environmental-pollution problem, reach the directional freeze refining effect by easy device, and then improve product quality, reduce production costs, be suitable for scale operation.
Description of drawings
Fig. 1 is a structural representation of the present invention;
Fig. 2 overlooks the direction synoptic diagram for composite die unitized construction of the present invention.
As shown in the figure: the thin polycrystalline ceramic fiber layer of muff 3-lower shoe track vehicle frame 4-composite die 5-suspension ring 6-steel bonnet 7-polycrystalline ceramic fiber layer 8-crystal whisker of hexa potassium titanate layer 9-corundum top board 10-steel boiler clothing 11-polycrystalline ceramic fiber layer 12-crystal whisker of hexa potassium titanate layer 13-corundum top board 14-rail wheel 15-steel substrate 16-graphite base plate 17-corundum riser 18-silicon-carbide particle 19-20-sealing ring 21-quick-speed jigs 22-sealing ring 23-heat-conducting plate among the upper insulation cover 2-of 1-
24-water-cooled copper dish 25-thermopair
Embodiment
The specific embodiment of the present invention is as follows:
As depicted in figs. 1 and 2, this device is cuboid, comprise insulation cover (1), middle muff (2) and lower shoe track vehicle frame (3), composite die (4), heat-conducting plate (23) and water-cooled copper dish (24), water-cooled copper dish (24) is located at the centre of lower shoe track vehicle frame (3), heat-conducting plate (23) is located at the top of water-cooled copper dish (24), composite die (4) is arranged at the top of heat-conducting plate (23), filled the silicon-carbide particle (18) of support and insulation effect around the composite die (4), between last insulation cover (1) and the middle muff (2) sealing-ring (20) has been arranged.
Last insulation cover (1) comprises suspension ring (5), steel bonnet (6), polycrystalline ceramic fiber layer (7), crystal whisker of hexa potassium titanate layer (8), corundum top board (9), outermost layer is steel bonnet (6), innermost layer is equipped with corundum top board (9), middle polycrystalline ceramic fiber layer (7) and the crystal whisker of hexa potassium titanate layer (8) settled is equipped with suspension ring (5) on the top board of steel bonnet (6).
Middle muff (2) comprises steel boiler clothing (10), polycrystalline ceramic fiber layer (11), crystal whisker of hexa potassium titanate layer (12), corundum side plate (13), outermost layer is steel boiler clothing (10), innermost layer is equipped with corundum side plate (13), middle polycrystalline ceramic fiber layer (11) and the crystal whisker of hexa potassium titanate layer (12) settled.Crystal whisker of hexa potassium titanate layer (8) or crystal whisker of hexa potassium titanate layer (12) adopt the former powder of crystal whisker of hexa potassium titanate sneak into the certain amount of bonding agent ram build up type, dry, slowly roasting is made.The polycrystalline ceramic fiber layer adopts the thickness of 10-20 millimeter.Being provided with thin polycrystalline ceramic fiber layer (19) between corundum side plate (13) and the corundum top board (9) and between potassium titanate crystal whisker layer (12) and the sealing-ring (20), in order to strengthen the sealing function between two component.
Lower shoe track vehicle frame (3) is provided with 4 rail wheels (14), and rail wheel (14) is installed on the steel substrate (15), and water-cooled copper dish (24) is placed in the centre of lower shoe track vehicle frame (3).Between steel substrate (15) and the middle muff (2) sealing-ring (22) is arranged.Between last insulation cover (1) and the middle muff (2); Quick-speed jigs (21) is installed, the tight seal in fitted seal circle (20) and (22) reinforcement between insulation cover (1), middle muff (2) and the lower shoe track vehicle frame (3) between middle muff (2) and the steel substrate (15).
Composite die (4) comprises graphite base plate (16) and corundum riser (17), and places the top of heat-conducting plate (23), has filled the silicon-carbide particle of support and insulation effect all around, and this particle sub-circular, granularity are the 4-8 millimeter.Surface-coated one deck silicon nitride releasing agent of composite die (4), the thickness of coating is 0.5～1.2mm.The middle part of heat-conducting plate (23) and water-cooled copper dish (24) is equipped with thermopair (25).
Use when of the present invention, in order to reach the purpose of directional freeze removal of impurities, workflow of the present invention is:
1. according to accompanying drawing structure assembled device, composite die (4) internal surface spraying one deck silicon nitride, being heated by resistive mode (as: globars, Si-Mo rod) toasts, make silicon nitride powder and composite die adherent close and firm, the body of heater of preheating simultaneously, be warming up to 800～1000 ℃, be pushed into the casting station.
2. open insulation cover (1), will pour in the sky composite die through the liquid metalluragical silicon of molten refined, the temperature that requires liquid metalluragical silicon is greater than 1600 ℃, and box is gone up insulation cover well rapidly, and quick-speed jigs (21) is clamped, and quick and stable is pushed into solidifies station.
3. the rapid-acting coupling of grafting water-cooled copper dish (24) guarantees that inlet and outlet pipe is unimpeded; Connect thermopair power supply signal line, accurately control the water-flowing amount of water-chilling plant by pilot circuit, silicon liquid carries out directional freeze, and solidification rate is controlled at 8～16mm/h.
4. after solidifying end, thermopair (25) temperature is reduced to below 300 ℃ and can be opened insulation cover, quickens to be cooled to room temperature, by muff (2) in suspension ring (5) lifting, collects silicon-carbide particle, removes the composite die side plate, takes out silicon ingot.
5. by reaching the bottom surface cleaning around the polishing silicon ingot, band-saw diamond or scroll saw excise impurity enriched district, silicon ingot top, and the excision amount is 10～15% of a silicon ingot height overall, promptly obtains high-quality metalluragical silicon silicon ingot.
Claims (8)
1. energy saver that is used for the removal of impurities of metalluragical silicon directional freeze, this device is cuboid, it is characterized in that this device comprises insulation cover (1), middle muff (2) and lower shoe track vehicle frame (3), composite die (4), heat-conducting plate (23) and water-cooled copper dish (24), water-cooled copper dish (24) is located at the centre of lower shoe track vehicle frame (3), heat-conducting plate (23) is located at the top of water-cooled copper dish (24), composite die (4) is arranged at the top of heat-conducting plate (23), filled the silicon-carbide particle of support and insulation effect around the composite die (4), between last insulation cover (1) and the middle muff (2) sealing-ring (20) has been arranged.
2. a kind of energy saver that is used for the removal of impurities of metalluragical silicon directional freeze according to claim 1, it is characterized in that the described insulation cover (1) of going up comprises suspension ring (5), steel bonnet (6), polycrystalline ceramic fiber layer (7), crystal whisker of hexa potassium titanate layer (8), corundum top board (9), outermost layer is steel bonnet (6), innermost layer is equipped with corundum top board (9), middle polycrystalline ceramic fiber layer (7) and the crystal whisker of hexa potassium titanate layer (8) settled is equipped with suspension ring (5) on the top board of steel bonnet (6).
3. a kind of energy saver that is used for the removal of impurities of metalluragical silicon directional freeze according to claim 1, its feature muff (2) in described comprises steel boiler clothing (10), polycrystalline ceramic fiber layer (11), crystal whisker of hexa potassium titanate layer (12), corundum side plate (13), outermost layer is steel boiler clothing (10), innermost layer is equipped with corundum side plate (13), middle polycrystalline ceramic fiber layer (11) and the crystal whisker of hexa potassium titanate layer (12) settled.
4. a kind of energy saver that is used for the removal of impurities of metalluragical silicon directional freeze according to claim 1, its feature is provided with 4 rail wheels (14) at described lower shoe track vehicle frame (3), rail wheel (14) is installed on the steel substrate (15), and water-cooled copper dish (24) is placed in the centre of lower shoe track vehicle frame (3).
5. a kind of energy saver that is used for the removal of impurities of metalluragical silicon directional freeze according to claim 1, its feature comprises graphite base plate (16) and corundum riser (17) at described composite die (4), and place the top of heat-conducting plate (23), filled the silicon-carbide particle of support and insulation effect all around, this particle sub-circular, granularity are the 4-8 millimeter.
6. a kind of energy saver that is used for the removal of impurities of metalluragical silicon directional freeze according to claim 1, its feature is equipped with thermopair (25) at the middle part of described heat-conducting plate (23) and water-cooled copper dish (24).
7. according to claim 2 and 3 described a kind of energy savers that are used for the removal of impurities of metalluragical silicon directional freeze, its feature described crystal whisker of hexa potassium titanate layer (8) or crystal whisker of hexa potassium titanate layer (12) adopt the former powder of crystal whisker of hexa potassium titanate sneak into the certain amount of bonding agent ram build up type, dry, slowly roasting is made.
8. according to claim 1 and 5 described a kind of energy savers that are used for the removal of impurities of metalluragical silicon directional freeze, its feature is at surface-coated one deck silicon nitride releasing agent of described composite die (4).
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| CN 201110152836 CN102259867B (en) | 2011-06-09 | 2011-06-09 | Energy saving device for directional solidification and impurity removal of metallurgical silicon |
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| CN 201110152836 CN102259867B (en) | 2011-06-09 | 2011-06-09 | Energy saving device for directional solidification and impurity removal of metallurgical silicon |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103395789A (en) * | 2013-08-06 | 2013-11-20 | 青岛隆盛晶硅科技有限公司 | Preliminary directional solidification process after polysilicon medium melting |
| CN103539126A (en) * | 2013-10-30 | 2014-01-29 | 大连理工大学 | Rapid freezing method of polycrystalline silicon |
| CN106164389A (en) * | 2014-06-25 | 2016-11-23 | 哈里伯顿能源服务公司 | It is associated with the heat insulation sealing cover of rigidity heat-barrier material |
| CN106232912A (en) * | 2014-06-25 | 2016-12-14 | 哈里伯顿能源服务公司 | There is the heat insulation sealing cover of change thermal characteristics |
| CN107513762A (en) * | 2016-06-16 | 2017-12-26 | 陕西盛华冶化有限公司 | A kind of metal-silicon furnace directional solidification reactor and pouring procedure |
| CN108437154A (en) * | 2018-04-16 | 2018-08-24 | 西安建筑科技大学 | Freezing casting prepares the mold that uniform orientation freezing can be achieved in porous ceramics technique |
| CN110355917A (en) * | 2019-07-25 | 2019-10-22 | 马鞍山纽泽科技服务有限公司 | A kind of mold heating device |
| CN112694065A (en) * | 2021-01-29 | 2021-04-23 | 华油惠博普科技股份有限公司 | Crude sulfur dehydration purification process and device |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103395789A (en) * | 2013-08-06 | 2013-11-20 | 青岛隆盛晶硅科技有限公司 | Preliminary directional solidification process after polysilicon medium melting |
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| CN103539126A (en) * | 2013-10-30 | 2014-01-29 | 大连理工大学 | Rapid freezing method of polycrystalline silicon |
| CN103539126B (en) * | 2013-10-30 | 2016-04-13 | 大连理工大学 | A kind of polysilicon quick setting method |
| CN106164389A (en) * | 2014-06-25 | 2016-11-23 | 哈里伯顿能源服务公司 | It is associated with the heat insulation sealing cover of rigidity heat-barrier material |
| CN106232912A (en) * | 2014-06-25 | 2016-12-14 | 哈里伯顿能源服务公司 | There is the heat insulation sealing cover of change thermal characteristics |
| CN107513762A (en) * | 2016-06-16 | 2017-12-26 | 陕西盛华冶化有限公司 | A kind of metal-silicon furnace directional solidification reactor and pouring procedure |
| CN107513762B (en) * | 2016-06-16 | 2024-01-09 | 陕西盛华冶化有限公司 | Directional solidification reactor of industrial silicon electric furnace and casting method |
| CN108437154A (en) * | 2018-04-16 | 2018-08-24 | 西安建筑科技大学 | Freezing casting prepares the mold that uniform orientation freezing can be achieved in porous ceramics technique |
| CN110355917A (en) * | 2019-07-25 | 2019-10-22 | 马鞍山纽泽科技服务有限公司 | A kind of mold heating device |
| CN112694065A (en) * | 2021-01-29 | 2021-04-23 | 华油惠博普科技股份有限公司 | Crude sulfur dehydration purification process and device |
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| CN102259867B (en) | 2012-12-12 |
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Effective date of registration: 20190329 Address after: 751100 Jinji Industrial Park, Wuzhong City, Ningxia Hui Autonomous Region, south of Jinwei Third Road Patentee after: Ningxia High Energy Technology Co., Ltd. Address before: 751100 Friendship East Road, Litong District, Wuzhong City, Ningxia Hui Autonomous Region Patentee before: Ningxia Yinxing Polycrystalline Silicon Co., Ltd. |
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