CN202968136U - Equipment for purification of polycrystalline silicon through rotating and air blowing induced inverse solidification - Google Patents
Equipment for purification of polycrystalline silicon through rotating and air blowing induced inverse solidification Download PDFInfo
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- CN202968136U CN202968136U CN 201220686761 CN201220686761U CN202968136U CN 202968136 U CN202968136 U CN 202968136U CN 201220686761 CN201220686761 CN 201220686761 CN 201220686761 U CN201220686761 U CN 201220686761U CN 202968136 U CN202968136 U CN 202968136U
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Abstract
The utility model belongs to the technical field of metallurgical purification, and in particular relates to equipment for purification of polycrystalline silicon through rotating and air blowing induced inverse solidification. The equipment is movably arranged at the bottom of a vacuum chamber through a water cooling disc; a graphite plate is arranged at the top end of the water cooling disc; a hole is arranged on the graphite plate; one end of a graphite supporting pillar is embedded and connected with the graphite plate through the hole, and the other end is embedded and connected with a graphite tray; a crucible is arranged on the graphite tray; a graphite heating body is sleeved on the periphery of the crucible; a carbon felt insulating barrel is sleeved outside the graphite heating body; a carbon felt insulating cover is provided with a hole, and is arranged at the top end of the carbon felt insulating barrel; an induction coil is sleeved outside the carbon felt insulating barrel; an air blowing pipeline is movably arranged at the top end of the vacuum chamber; and the air blowing port of the air blowing pipeline is arranged in the center of the upper part of the crucible. The equipment disclosed by the utility model, on the basis of original directional solidification equipment, is added with crucible rotating and air blowing functions, and the equipment is convenient to modify and install, simple to operate, capable of effectively removing impurities enriched on the tail of an ingot, saving production cycle and cost, and is applicable to industrial mass production.
Description
Technical field
The utility model belongs to the metallurgy purification technical field, particularly a kind of equipment of inducing the reverse solidification purifying polycrystalline silicon.
Background technology
The development of photovoltaic industry depends on the purification to the silicon raw material, in the process that the silicon raw material is purified, directional solidification process is most important to removing the metallic impurity that in the silicon raw material, segregation coefficient is very little, it is one of present solar-grade polysilicon effective means of purifying, in addition, directional solidification technique is widely used in metallurgy purification.Directional freeze is to adopt compulsory means to form the thermograde of specific direction in melt, make the melt crystallization nucleation at the low position of temperature, at first the starting point that becomes melt solidifying solidifies, existence due to thermograde, melt solidifies along the opposite direction of hot-fluid, obtains to have the column crystal of specific orientation.It is to utilize the different solubility of impurity element in melt and solid that directional freeze is purified, the impurity element that segregation coefficient is less in process of setting is pushed to the solid-liquid interface forward position, constantly enrichment in melt, and the afterbody at ingot casting solidifies at last, with the excision of ingot casting afterbody, can reach the purpose of purification.
yet, ingot casting is solidifying coda, impurity enriched is in the melt at crucible top, in the end in the slow solidification process, the position that foreign matter content is high can be to the low position diffusion of foreign matter content, make silicon purity reduce gradually along with the prolongation of soaking time, this has affected refining effect, and in this case, the afterbody waste material of excision is up to 25% ~ 35%, be that yield rate only is 65-75%, and the hardness ratio of silicon ingot is larger, need high-power cutting facility silicon ingot and the high ingot casting tailing of afterbody foreign matter content of purifying could be separated, the general method of line cutting and the cutting of diamond saw band of using is cut at present, but the cutting facility cost is high, saw band consumption is large, be unfavorable for the reduction of industrial production cost, and domestic rarely seen fruitful method facilitates the removal of tailing.
The utility model content
the present invention seeks to as overcoming above deficiency, proposed a kind of rotation and blown and induce the equipment of reverse solidification purifying polycrystalline silicon, this equipment is simple, easy and simple to handle, cost is lower, and being beneficial to the high ingot casting tailing of foreign matter content is removed quickly and easily, solidifying coda, make crucible rotation and be blown into a certain amount of high purity inert gas, molten silicon is assembled and rapid reverse solidification to crucible wall under the dual function of centrifugal force and air-flow, reduced the back diffusion of impurity, improved the yield of ingot casting, solidifying reverse solidification that ending phase realizes the impurity enriched district and separating.
the technical scheme that adopts for achieving the above object is: the equipment of reverse solidification purifying polycrystalline silicon is induced in a kind of rotation and air blowing, consist of outer wall by vacuum chamber, vacuum-lines is installed on outer wall, vacuum-lines one end is connected with the vacuum pump group, it is characterized in that: aqueous cold plate is movably installed in chamber bottom, graphite cake is placed in the aqueous cold plate top, have the hole on graphite cake, graphite pillar one end is connected by hole and graphite cake are nested, the other end is connected with the graphite pallet is nested, crucible is placed on the graphite pallet, graphite heater is placed in the crucible periphery and is fixed on the vacuum chamber sidewall, carbon felt insulated tank is placed in outside graphite heater and is fixed on the vacuum chamber sidewall, have the hole on carbon felt insulation cover, and be placed in carbon felt insulated tank top, ruhmkorff coil is placed in outside carbon felt insulated tank, and be fixed on the vacuum chamber sidewall, the air blowing pipeline is movably installed in the vacuum chamber top, the puff port of air blowing pipeline is positioned at central position directly over crucible.
Hole on described graphite cake is at least 3.
Have draw-in groove on described graphite pallet.
Between described air blowing pipeline and vacuum chamber, vacuum-sealing is flexibly connected, and its puff port is apart from 5-15cm directly over crucible.
Equipment of the present utility model is to increase the function of crucible rotation and air blowing on the basis of original apparatus for directional solidification, scrap build is easy for installation, and is simple to operate, can effectively remove the impurity of ingot casting afterbody enrichment, save production cycle and cost, be applicable to large-scale industrialization production.
The unusual effect that uses equipment of the present utility model to produce acquisition is: when melt solidifying to impurity phase during to the silicon ingot top of concentrating, the beginning rotating crucible, be blown into rare gas element from the crucible top to the foreign matter content of final set higher silicon melt center simultaneously, make this part silicon melt assemble and rapid reverse solidification to crucible wall under the dual function of centrifugal force and air-flow, impurity is pinned among the ingot casting of upper strata, reduced the back diffusion of impurity, improved the yield of ingot casting, yield rate reaches 80%-95%; And it is higher to solidify rear upper strata silicon ingot foreign matter content, the centre is thinner, and both sides are thicker, and lower floor's silicon ingot is to obtain by slow directional freeze, foreign matter content is very low, different from the crystal orientation of lower floor directionally solidified silicon ingots crystal grain due to the upper strata silicon ingot, density is not identical yet, the bonding force between two-layer silicon ingot a little less than, can separate by the mode of beaing, reduce the consumption of line cutting and the cutting of diamond saw band, reduced process procedure, reduced energy consumption.
Description of drawings
The device structure schematic diagram of reverse solidification purifying polycrystalline silicon is induced in a kind of rotation of Fig. 1 and air blowing
In figure: (1) air blowing pipeline, (2) vacuum chamber, (3) carbon felt insulation cover, (4) carbon felt insulated tank, (5) ruhmkorff coil, (6) graphite heater, (7) crucible, (8) molten silicon liquid, (9) graphite pallet, (10) graphite pillar, (11) graphite cake, (12) aqueous cold plate, (13) vacuum-lines, (14) vacuum pump group
Embodiment
Describe the present invention in detail below in conjunction with specific embodiments and the drawings, but the present invention is not limited to specific embodiment.
Embodiment 1
the equipment that the reverse solidification purifying polycrystalline silicon is induced in a kind of rotation as shown in Figure 1 and air blowing, consist of outer wall by vacuum chamber 2, vacuum-lines 13 is installed on outer wall, vacuum-lines 13 1 ends are connected with vacuum pump group 14, be used for vacuum chamber is vacuumized, aqueous cold plate 12 movable sealings are installed on vacuum chamber 2 bottoms, its inside is equipped with cooling water pipeline, realization is cooling to aqueous cold plate, graphite cake 11 is placed in the aqueous cold plate top, have the hole on graphite cake 11, graphite pillar 10 1 ends are connected with graphite cake 11 is nested by the hole, the other end is connected with graphite pallet 9 is nested, crucible 7 is placed on graphite pallet 9, graphite heater 6 is placed in the crucible periphery and is fixed on vacuum chamber 2 sidewalls, carbon felt insulated tank 4 is placed in outside graphite heater 6 and is fixed on vacuum chamber 2 sidewalls, carbon felt insulation cover 3 is placed in carbon felt insulated tank 4 tops, prevent that foreign material from falling among crucible, ruhmkorff coil 5 is placed in outside carbon felt insulated tank 4, and be fixed on vacuum chamber 2 sidewalls, air blowing pipeline 1 is fixedly installed in vacuum chamber 2 tops, and the puff port of air blowing pipeline 1 is positioned at center directly over crucible.
Have the hole on carbon felt insulation cover 3, between carbon felt insulation cover 3 and carbon felt insulated tank 4, carbon felt insulation cover 3 is all non-being tightly connected with air blowing pipeline 1, is beneficial to the rare gas element that is blown into and is taken away by the vacuum pump group.
Hole on graphite cake 11 is 4.
Have draw-in groove on graphite pallet 9, be used for crucible is carried out screens and fixing.
Between air blowing pipeline 1 and vacuum chamber 2, vacuum-sealing is fixedly connected with, and to guarantee the vacuum tightness of vacuum chamber, its puff port guarantees that apart from crucible 10cm air-flow steadily blows at the upper strata bath surface.
Embodiment 2
Adopt the described equipment of embodiment 1 to induce the reverse solidification purifying polycrystalline silicon, at first add the silicon material of cleaning of crucible volume 95% in the crucible 7, purity is 99.5%, opens afterwards vacuum pump group 14 vacuum tightnesss in vacuum chamber 2 are extracted into 5Pa;
the second step melting, solidify: power-on, utilize ruhmkorff coil 5 and graphite heater 6 that the silicon material in crucible 7 is heated to 1450 ℃ to being fused into silicon melt fully, and be incubated 30min at this temperature, pull vertically downward aqueous cold plate 12, make silicon melt in crucible 7 with the speed of 2mm/min uniform motion vertically downward, draw ingot, silicon melt carries out directional freeze by crucible 7 bottoms to the top, when silicon melt is solidified to 80%, rotating water cold dish 12, make crucible 7 with the speed rotation of 30r/min, make upper strata excess silicon melt assemble to crucible 7 sidewalls under the effect of centrifugal force, be blown into simultaneously purity to center, excess silicon melt top, upper strata and be 99.91% argon gas, the speed that is blown into is 8m/s, temperature when being blown into is 15 ℃, make upper strata excess silicon melt under the effect of air-flow from crucible 7 the mind-set sidewall assemble and reverse solidification rapidly, solidify fully in crucible 7 side-walls at last.
The 3rd step aftertreatment: stopped heating, until the cooling rear taking-up of whole silicon ingot, in removal, crucible 7 sidewalls solidify the ingot casting of the impurity enriched that obtains, and remaining lower floor ingot casting is the HIGH-PURITY SILICON ingot casting, and its purity will reach 99.99%, and yield rate reaches 80%.
Embodiment 3
Adopt the described equipment of embodiment 1 to induce the reverse solidification purifying polycrystalline silicon, at first add the silicon material of cleaning of crucible volume 93% in the crucible 7, purity is 99.7%, opens afterwards vacuum pump group 14 vacuum tightnesss in vacuum chamber 2 are extracted into 2Pa;
the second step melting, solidify: power-on, utilize ruhmkorff coil 5 and graphite heater 6 that the silicon material in crucible 7 is heated to 1500 ℃ to being fused into silicon melt fully, and be incubated 45min at this temperature, pull vertically downward aqueous cold plate 12, make silicon melt in crucible 7 with the speed of 0.8mm/min uniform motion vertically downward, draw ingot, silicon melt carries out directional freeze by crucible 7 bottoms to the top, when silicon melt is solidified to 85%, rotating water cold dish 12, make crucible 7 with the speed rotation of 40r/min, make upper strata excess silicon melt assemble to crucible 7 sidewalls under the effect of centrifugal force, be blown into simultaneously purity to center, excess silicon melt top, upper strata and be 99.94% argon gas, the speed that is blown into is 25m/s, temperature when being blown into is 10 ℃, make excess silicon melt mind-set sidewall from crucible 7 in upper strata assemble and rapid reverse solidification, solidify fully in crucible 7 side-walls at last.
The 3rd step aftertreatment: stopped heating, until the cooling rear taking-up of whole silicon ingot, in removal, crucible 7 sidewalls solidify the ingot casting of the impurity enriched that obtains, and remaining lower floor ingot casting is the HIGH-PURITY SILICON ingot casting, and its purity will reach 99.995%, and yield rate reaches 91%.
Embodiment 4
Adopt the described equipment of embodiment 1 to induce the reverse solidification purifying polycrystalline silicon, at first add the silicon material of cleaning of crucible volume 90% in the crucible 7, purity is 99.9%, opens afterwards vacuum pump group 14 vacuum tightnesss in vacuum chamber 2 are extracted into 0.1Pa;
the second step melting, solidify: power-on, utilize ruhmkorff coil 5 and graphite heater 6 that the silicon material in crucible 7 is heated to 1650 ℃ to being fused into silicon melt fully, and be incubated 60min at this temperature, pull vertically downward aqueous cold plate 12, make silicon melt in crucible 7 with the speed of 0.1mm/min uniform motion vertically downward, draw ingot, silicon melt carries out directional freeze by crucible 7 bottoms to the top, when silicon melt is solidified to 95%, rotating water cold dish 12, make crucible 7 with the speed rotation of 50r/min, make upper strata excess silicon melt assemble to crucible 7 sidewalls under the effect of centrifugal force, be blown into simultaneously purity to center, excess silicon melt top, upper strata and be 99.97% argon gas, the speed that is blown into is 40m/s, temperature when being blown into is 5 ℃, make excess silicon melt mind-set sidewall from crucible 7 in upper strata assemble and rapid reverse solidification, solidify fully in crucible 7 side-walls at last.
The 3rd step aftertreatment: stopped heating, until the cooling rear taking-up of whole silicon ingot, in removal, crucible 7 sidewalls solidify the ingot casting of the impurity enriched that obtains, and remaining lower floor ingot casting is the HIGH-PURITY SILICON ingot casting, and its purity will reach 99.999%.Yield rate reaches 95%.
Claims (4)
1. one kind is rotated and blows the equipment of reverse solidification purifying polycrystalline silicon of inducing, consist of outer wall by vacuum chamber (2), vacuum-lines (13) is installed on outer wall, vacuum-lines (13) one ends are connected with vacuum pump group (14), it is characterized in that: aqueous cold plate (12) is movably installed in bottom vacuum chamber (2), graphite cake (11) is placed in the aqueous cold plate top, graphite cake has the hole on (11), graphite pillar (10) one ends are by hole and nested connection of graphite cake (11), the other end and nested connection of graphite pallet (9), crucible (7) is placed on graphite pallet (9), graphite heater (6) is placed in the crucible periphery and is fixed on vacuum chamber (2) sidewall, carbon felt insulated tank (4) is placed in outside graphite heater (6) and is fixed on vacuum chamber (2) sidewall, have the hole on carbon felt insulation cover (3), and be placed in carbon felt insulated tank (4) top, ruhmkorff coil (5) is placed in outside carbon felt insulated tank (4), and be fixed on vacuum chamber (2) sidewall, air blowing pipeline (1) is movably installed in vacuum chamber (2) top, the puff port of air blowing pipeline (1) is positioned at central position directly over crucible.
2. the equipment of reverse solidification purifying polycrystalline silicon is induced in a kind of rotation according to claim 1 and air blowing, and it is characterized in that: the hole on described graphite cake (11) is at least 3.
3. the equipment of reverse solidification purifying polycrystalline silicon is induced in a kind of rotation according to claim 1 and air blowing, it is characterized in that: have draw-in groove on described graphite pallet (9).
4. the equipment of reverse solidification purifying polycrystalline silicon is induced in a kind of rotation according to claim 1 and air blowing, and it is characterized in that: between described air blowing pipeline (1) and vacuum chamber (2), vacuum-sealing is flexibly connected, and its puff port is apart from 5-15cm directly over crucible.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201220686761 CN202968136U (en) | 2012-12-13 | 2012-12-13 | Equipment for purification of polycrystalline silicon through rotating and air blowing induced inverse solidification |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201220686761 CN202968136U (en) | 2012-12-13 | 2012-12-13 | Equipment for purification of polycrystalline silicon through rotating and air blowing induced inverse solidification |
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| CN202968136U true CN202968136U (en) | 2013-06-05 |
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| CN 201220686761 Withdrawn - After Issue CN202968136U (en) | 2012-12-13 | 2012-12-13 | Equipment for purification of polycrystalline silicon through rotating and air blowing induced inverse solidification |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102976335A (en) * | 2012-12-13 | 2013-03-20 | 青岛隆盛晶硅科技有限公司 | Method and apparatus for purifying polycrystalline silicon through rotation and blow induced inversion solidification |
| CN103539126A (en) * | 2013-10-30 | 2014-01-29 | 大连理工大学 | Rapid freezing method of polycrystalline silicon |
| CN103541003A (en) * | 2013-11-14 | 2014-01-29 | 乐山新天源太阳能科技有限公司 | Polysilicon ingot furnace |
| CN103556220A (en) * | 2013-11-14 | 2014-02-05 | 乐山新天源太阳能科技有限公司 | Polycrystalline silicon ingot furnace |
| CN109133068A (en) * | 2018-11-19 | 2019-01-04 | 成都斯力康科技股份有限公司 | Metallurgy method removal of impurities prepares the device and method of solar-grade silicon ingot |
| CN109354024A (en) * | 2018-11-19 | 2019-02-19 | 成都斯力康科技股份有限公司 | A kind of device and method of infant industry silicon separation, impurity removal |
-
2012
- 2012-12-13 CN CN 201220686761 patent/CN202968136U/en not_active Withdrawn - After Issue
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102976335A (en) * | 2012-12-13 | 2013-03-20 | 青岛隆盛晶硅科技有限公司 | Method and apparatus for purifying polycrystalline silicon through rotation and blow induced inversion solidification |
| CN102976335B (en) * | 2012-12-13 | 2014-04-30 | 青岛隆盛晶硅科技有限公司 | Method and apparatus for purifying polycrystalline silicon through rotation and blow induced inversion solidification |
| 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 |
| CN103541003A (en) * | 2013-11-14 | 2014-01-29 | 乐山新天源太阳能科技有限公司 | Polysilicon ingot furnace |
| CN103556220A (en) * | 2013-11-14 | 2014-02-05 | 乐山新天源太阳能科技有限公司 | Polycrystalline silicon ingot furnace |
| CN103556220B (en) * | 2013-11-14 | 2016-06-08 | 乐山新天源太阳能科技有限公司 | Polycrystalline silicon ingot or purifying furnace |
| CN103541003B (en) * | 2013-11-14 | 2016-08-17 | 乐山新天源太阳能科技有限公司 | Polycrystalline silicon ingot or purifying furnace |
| CN109133068A (en) * | 2018-11-19 | 2019-01-04 | 成都斯力康科技股份有限公司 | Metallurgy method removal of impurities prepares the device and method of solar-grade silicon ingot |
| CN109354024A (en) * | 2018-11-19 | 2019-02-19 | 成都斯力康科技股份有限公司 | A kind of device and method of infant industry silicon separation, impurity removal |
| CN109133068B (en) * | 2018-11-19 | 2021-06-22 | 成都斯力康科技股份有限公司 | Device and method for preparing solar-grade silicon ingot by removing impurities through metallurgy method |
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| C14 | Grant of patent or utility model | ||
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| AV01 | Patent right actively abandoned |
Granted publication date: 20130605 Effective date of abandoning: 20140430 |
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| RGAV | Abandon patent right to avoid regrant |