CN102976334B - Method and equipment for rapid collection and purification of polycrystalline silicon through directional solidification of tailing - Google Patents
Method and equipment for rapid collection and purification of polycrystalline silicon through directional solidification of tailing Download PDFInfo
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- CN102976334B CN102976334B CN201210537364.4A CN201210537364A CN102976334B CN 102976334 B CN102976334 B CN 102976334B CN 201210537364 A CN201210537364 A CN 201210537364A CN 102976334 B CN102976334 B CN 102976334B
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Abstract
The invention belongs to the technical field of metallurgy purification, and particularly relates to a method and equipment for directional solidification and purification of polycrystalline silicon through taking tailing. According to the method, under the inert gas shielding environment, abluent silicon is heated to be fully melted so as to carry out directional solidification; ingot pulling is stopped when solidification is completed by 85-90%, a graphite bent pipe is stretched into surplus unset silicon at the upper layer, then the other end of the graphite bent pipe is vacuumed through a vacuum unit, so that the surplus unset silicon at the upper layer enters the graphite bent pipe under the action of pressure difference and enters a water cooling collection box through the guide of the graphite bent pipe; heating is stopped after all the surplus unset silicon at the upper layer enters the water cooling collection box, and cast ingot solidified in a crucible is silicon cast ingot of high purity. Due to the method, back-diffusion of impurity is prevented, technology processes are reduced, and the yield of cast ingot is improved. The equipment is convenient to improve and install, and a tailing collection device can be used repeatedly, can collect more tailings, and is safe and reliable.
Description
Technical field
The invention belongs to metallurgy purification technical field, particularly a kind of method and apparatus of tailing taking-out type directional solidification purified polysilicon.
Background technology
The purification of silicon raw material is the important step of photovoltaic industrial chain, and the fast development of photovoltaic industry depends on high-level efficiency, method of purification cheaply.Directional solidification technique has been widely used in the numerous areas of purification of metals, has obtained significant effect.In the process that silicon raw material is purified, segregation coefficient can, to enrichment in liquid phase, finally be removed in directional freeze process much smaller than 1 metallic impurity.This method is that current metallurgy method is prepared one of key link of solar-grade polysilicon, is the effective means of removing metallic impurity in polysilicon.The principle of directional freeze is to adopt compulsory means in melt, to form the thermograde of specific direction, the position that in silicon melt, temperature is lower becomes first crystallization nucleation of forming core source, become the starting point of melt solidifying and start growth, existence due to unidirectional thermograde, melt is constantly grown along the direction contrary with hot-fluid, the final column crystal with specific orientation that forms.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 discharged from and enters in liquid phase in forward position, solid-liquid interface place, and constantly enrichment in melt, finally the afterbody at ingot casting solidifies, by the higher region excision of ingot casting afterbody impurity concentration, can obtain the ingot casting of low-metal content, and then reach the object of purification.
Yet, solidifying latter stage, along with the continuous enrichment of impurity and constantly reducing of melt volume, the concentration of impurity can be more and more higher, and the impurity of high density is retained in the region of final set.In slow cooling process subsequently, the impurity of area with high mercury can spread to low concentration region, make silicon purity along with the prolongation of soaking time reduces on the contrary gradually, this has affected refining effect, and in this case, need cut afterbody waste material up to 25%～35%, yield rate is only 65-75%.Simultaneously, because the hardness ratio of silicon is larger, need high-power cutting facility the silicon ingot of purification and the high ingot casting tailing of afterbody foreign matter content could be separated, the general method of line cutting and the cutting of diamond saw band of using is cut at present, but cutting facility cost is high, saw band consumption is large, is unfavorable for the reduction of industrial production cost, at present, domestic rarely seen fruitful method facilitates the removal of tailing.
Summary of the invention
The present invention seeks to as overcoming above deficiency, a kind of method of directional freeze tailing quick collection purifying polycrystalline silicon has been proposed, solidifying latter stage, graphite bend pipe is stretched among the silicon melt that the not solidified foreign matter content in upper strata is higher, the other end extracting vacuum at graphite bend pipe, the silicon melt that the not solidified foreign matter content in upper strata is high enters in graphite bend pipe under the effect of pressure difference, under the guiding of graphite guide tube, enter among water-cooled collection box, realize the directly separated of impurity enriched district and the HIGH-PURITY SILICON ingot casting having solidified solidifying ending phase, suppressed the back diffusion of impurity, the purity of polysilicon and the yield of ingot casting have been improved, reduced process procedure, the equipment that the method adopts has also been proposed in addition, this equipment is simple, easy and simple to handle, cost is lower, and being beneficial to the tailing that foreign matter content is high is removed quickly and easily.
The technical scheme that adopted is for achieving the above object: a kind of method of directional freeze tailing quick collection purifying polycrystalline silicon, is characterized in that: in protection of inert gas environment, clean silicon material is heated to melt completely after forming silicon melt is incubated; Lower the temperature afterwards, draw ingot vertically downward, carry out directional freeze; When having solidified 85～90%, stop drawing ingot, graphite bend pipe is stretched in the not solidified excess silicon melt in upper strata, afterwards with vacuum unit to graphite bend pipe the other end extracting vacuum, the not solidified excess silicon melt in upper strata enters in graphite bend pipe under pressure difference effect, and under the guiding of graphite guide tube, enters among water-cooled collection box; Until upper strata, not solidified excess silicon melt all imports after water-cooled collection box, cuts off the electricity supply, and stops heating, in water-cooled collection box, solidify obtain for tailing, in crucible, solidify the ingot casting obtaining and be HIGH-PURITY SILICON ingot casting.
The concrete steps of the method that adopts are as follows:
The first step pre-treatment: add the clean silicon material of crucible volume 90～95% in crucible, close vent line, open vacuum pump group, first the vacuum tightness in vacuum chamber is extracted into 0.01-10Pa, close afterwards vacuum pump group, open vent line, in vacuum chamber, be filled with rare gas element, reach 500～10000Pa to pressure, close vent line;
Second step melting, solidify: power-on, utilize ruhmkorff coil and graphite heater that the silicon material in crucible is heated to 1450～1650 ℃ to being fused into silicon melt completely, and be incubated 30～60min at this temperature, pull vertically downward aqueous cold plate, make silicon melt in crucible with the speed of 0.1-2mm/min uniform motion vertically downward, draw ingot, silicon melt is carried out directional freeze to top by crucible bottom, when silicon melt is solidified to 85～90%, stop drawing ingot, graphite bend pipe is moved down, its lower end extend in the not solidified excess silicon melt in upper strata, open valve, open vacuum unit, vacuum tightness in graphite bend pipe and graphite guide tube is evacuated to 1-500Pa, between graphite bend pipe and graphite guide tube and vacuum chamber, mineralization pressure is poor, the not solidified excess silicon melt in upper strata enters graphite bend pipe under pressure difference effect, and enter in cold-crucible under the guiding of graphite guide tube.
The 3rd step aftertreatment: treat that the not solidified excess silicon melt in upper strata all enters cold-crucible, cut off the electricity supply, stop heating, the tailing that is rich in impurity has just been collected among cold-crucible, after melting finishes, opens collection case lid, reclaim tailing, in crucible, solidifying the ingot casting obtaining is HIGH-PURITY SILICON ingot casting, and its purity will reach 99.99%-99.999%, and yield rate reaches 85-95%.
Described silicon material is industrial silicon, and its purity is 99.0%～99.9%.
Described rare gas element is argon gas or helium, and its purity is more than 99.9%.
The equipment that a kind of method of directional freeze tailing quick collection purifying polycrystalline silicon adopts, by vacuum chamber, form outer wall, vacuum-lines is installed on outer wall, vacuum-lines one end is connected with vacuum pump group, it is characterized in that: on outer wall, be installed with vent line, aqueous cold plate is movably installed in chamber bottom, graphite cake is placed in aqueous cold plate top, on graphite cake, have hole, graphite pillar one end is connected by hole and graphite cake are nested, the other end is connected with graphite pallet is nested, crucible is placed on graphite pallet, graphite heater is placed on crucible periphery and is fixed on vacuum chamber sidewall, carbon felt insulated tank is placed on outside graphite heater and is fixed on vacuum chamber sidewall, on carbon felt insulation cover, have hole, be placed in carbon felt insulated tank top, ruhmkorff coil is placed on outside carbon felt insulated tank, and be fixed on vacuum chamber sidewall, graphite bend pipe upper end is fixedly installed on expansion link, and its lower end is placed in central position directly over crucible through carbon felt insulation cover, graphite bend pipe upper end open place is tightly connected by junctor and graphite guide tube intermediate openings, graphite guide tube upper end air-tight movable is installed on vacuum chamber top, its upper end open is tightly connected by valve and vacuum withdraw device, the sealing of water-cooled collection box is fixedly installed on vacuum chamber sidewall, graphite bend pipe lower ending opening is connected with water-cooled collection box air-tight movable.
At least 3, hole on described graphite cake, has draw-in groove on graphite pallet.
Described graphite bend pipe is sharp mouth graphite bend pipe, and its lower end mouth of pipe is sharp mouth taper.
Described graphite guide tube middle part is installed with expansion link.
On described water-cooled collection box outer side wall, collection case lid is installed
Described vacuum withdraw device adopts bleed line air-tight movable to be installed on graphite guide tube upper end open, and vacuum unit is fixedly installed in the other end of bleed line, and vacuumometer is installed on bleed line.
The unusual effect of the inventive method is: when melt solidifying is to impurity phase during to concentrated silicon ingot top, utilize pressure difference that the high tailing of foreign matter content is collected in water-cooled collection box, so just reduced the back diffusion of impurity, improved the yield of ingot casting, yield reaches 85%-95%, reduce the consumption of line cutting and the cutting of diamond saw band, reduced process procedure, reduced energy consumption.
Equipment of the present invention is on the basis of original apparatus for directional solidification, to increase breather line, graphite bend pipe, graphite guide tube and water-cooled collection box, scrap build is easy for installation, simple to operate, can effectively remove the impurity of ingot casting afterbody enrichment, the not only recursive use of this tailing collection device, and the tailing amount that can collect is larger, and equipment safety is reliable, saved production cycle and cost, be applicable to large-scale industrialization and produce.
Accompanying drawing explanation
The equipment schematic diagram that the method for a kind of directional freeze tailing of Fig. 1 quick collection purifying polycrystalline silicon adopts
In figure: (1) graphite bend pipe, (2) vacuum chamber, (3) carbon felt insulation cover, (4) carbon felt insulated tank, (5) ruhmkorff coil, (6) graphite heater, (7) crucible, (8) solidify silicon ingot, (9) graphite pallet, (10) graphite pillar, (11) graphite cake, (12) aqueous cold plate, (13) vent line, (14) vacuum pump group, (15) vacuum-lines, (16) collect case lid, (17) water-cooled collection box, (18) graphite guide tube, (19) junctor, (20) valve, (21) bleed line, (22) expansion link, (23) vacuumometer, (24) vacuum unit
Embodiment
Below in conjunction with specific embodiments and the drawings, describe the present invention in detail, but the present invention is not limited to specific embodiment.
Embodiment 1
The equipment that a kind of directional freeze tailing quick collection purifying polycrystalline silicon as shown in Figure 1 adopts, by vacuum chamber 2, form outer wall, vacuum-lines 15 is installed on outer wall, and vacuum-lines 15 one end are connected with vacuum pump group 14, and vacuum pump group is used for vacuum chamber extracting vacuum.
On outer wall, be installed with vent line 13, vent line is for being filled with gas to vacuum chamber, as rare gas element etc., aqueous cold plate 12 is movably installed in vacuum chamber 2 bottoms, aqueous cold plate can be according to speed rising or the decline set under the effect of leading screw and motor, graphite cake 11 is placed in aqueous cold plate top, on graphite cake 11, have 4 holes, graphite pillar 10 one end are connected with graphite cake 11 is nested by hole, the other end is connected with graphite pallet 9 is nested, on graphite pallet, have draw-in groove, be beneficial to graphite pillar and be connected with the nested of its.
Crucible 7 is placed on graphite pallet 9, graphite heater 6 is placed on crucible periphery and is fixed on vacuum chamber 2 sidewalls, carbon felt insulated tank 4 is placed on outside graphite heater 6 and is fixed on vacuum chamber 2 sidewalls, on carbon felt insulation cover 3, have hole, be placed in carbon felt insulated tank 4 tops, ruhmkorff coil 5 is placed on outside carbon felt insulated tank 4, and is fixed on vacuum chamber 2 sidewalls.
Graphite bend pipe 1 upper end is fixedly installed on expansion link 22, and its lower end is placed in central position directly over crucible through carbon felt insulation cover 3, graphite bend pipe 1 upper end open place is tightly connected by junctor 19 and graphite guide tube 18 intermediate openings, graphite guide tube upper end air-tight movable is installed on vacuum chamber 2 tops, its upper end open is tightly connected by valve 20 and vacuum withdraw device, 17 sealings of water-cooled collection box are fixedly installed on vacuum chamber 2 sidewalls, and graphite bend pipe 1 lower ending opening is connected with water-cooled collection box 17 air-tight movables.
Graphite bend pipe 1 is sharp mouth graphite bend pipe, and its lower end mouth of pipe is sharp mouth taper, is beneficial to upper strata not solidified afterbody silicon material to be collected among water-cooled collection box
On water-cooled collection box 17 outer side walls, be provided with and collect case lid 16, in water-cooled collection box, collect after full tailing, can open after collecting case lid and take out and reclaim tailing.
Vacuum withdraw device adopts bleed line 21 air-tight movables to be installed on graphite guide tube upper end open, vacuum unit 24 is fixedly installed in the other end of bleed line, vacuumometer 23 is installed on bleed line, and this device is used for graphite guide tube and graphite bend pipe extracting vacuum.
Embodiment 2
Equipment described in employing embodiment 1 is got tailing and is carried out directional solidification purified polysilicon, first to adding the clean purity of crucible volume 90% in crucible 7, be 99.0% silicon material, close vent line 13, open vacuum pump group 15, the vacuum tightness in vacuum chamber 2 is extracted into 10Pa, close vacuum pump group 14, open vent line, in vacuum chamber 2, be filled with 99.91% argon gas, reach 500Pa to pressure, close vent line;
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 completely, and be incubated 30min at this temperature, pull vertically downward aqueous cold plate 12, make silicon melt in crucible 7 with the speed of 2.0mm/min uniform motion vertically downward, draw ingot, silicon melt carries out directional freeze by crucible 7 bottoms to top, when silicon melt is solidified to 85%, stop drawing ingot, graphite bend pipe 1 is moved down, its lower end extend in the not solidified excess silicon melt in upper strata, open valve 20, open vacuum unit 24, vacuum tightness in graphite bend pipe and graphite guide tube 18 is evacuated to 1Pa, between graphite bend pipe and graphite guide tube and vacuum chamber 2, mineralization pressure is poor, the not solidified excess silicon melt in upper strata enters graphite bend pipe under pressure difference effect, and enter in cold-crucible under the guiding of graphite guide tube 18.
The 3rd step aftertreatment: treat that the not solidified excess silicon melt in upper strata all enters cold-crucible, cut off the electricity supply, stop heating, the tailing that is rich in impurity has just been collected among cold-crucible, after melting finishes, opens collection case lid, reclaim tailing, in crucible, solidifying the ingot casting obtaining is HIGH-PURITY SILICON ingot casting, and its purity will reach 99.99%, and yield rate reaches 85%.
Embodiment 3
Equipment described in employing embodiment 1 is got tailing and is carried out directional solidification purified polysilicon, first to adding the clean purity of crucible volume 92% in crucible 7, be 99.3% silicon material, close vent line 13, open vacuum pump group 15, the vacuum tightness in vacuum chamber 2 is extracted into 2Pa, close vacuum pump group 14, open vent line, to being filled with purity in vacuum chamber 2, be 99.96% argon gas, reach 5000Pa to pressure, close vent line;
Second step melting, solidify: power-on, utilize ruhmkorff coil 5 and graphite heater 6 that the silicon material in crucible 7 is heated to 1550 ℃ to being fused into silicon melt completely, and be incubated 45min at this temperature, pull vertically downward aqueous cold plate 12, make silicon melt in crucible 7 with the speed of 1.0mm/min uniform motion vertically downward, draw ingot, silicon melt carries out directional freeze by crucible 7 bottoms to top, when silicon melt is solidified to 86%, stop drawing ingot, graphite bend pipe 1 is moved down, its lower end extend in the not solidified excess silicon melt in upper strata, open valve 20, open vacuum unit 24, vacuum tightness in graphite bend pipe and graphite guide tube 18 is evacuated to 200Pa, between graphite bend pipe and graphite guide tube and vacuum chamber 2, mineralization pressure is poor, the not solidified excess silicon melt in upper strata enters graphite bend pipe under pressure difference effect, and enter in cold-crucible under the guiding of graphite guide tube 18.
The 3rd step aftertreatment: treat that the not solidified excess silicon melt in upper strata all enters cold-crucible, cut off the electricity supply, stop heating, the tailing that is rich in impurity has just been collected among cold-crucible, after melting finishes, opens collection case lid, reclaim tailing, in crucible, solidifying the ingot casting obtaining is HIGH-PURITY SILICON ingot casting, and its purity will reach 99.996%, and yield rate reaches 91%.
Embodiment 4
Equipment described in employing embodiment 1 is got tailing and is carried out directional solidification purified polysilicon, first to adding the clean purity of crucible volume 95% in crucible 7, be 99.9% silicon material, close vent line 13, open vacuum pump group 14, the vacuum tightness in vacuum chamber 2 is extracted into 0.01Pa, close vacuum pump group 14, open vent line, to being filled with purity in vacuum chamber 2, be 99.95% helium, reach 10000Pa to pressure, close vent line;
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 completely, 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 top, when silicon melt is solidified to 90%, stop drawing ingot, graphite bend pipe 1 is moved down, its lower end extend in the not solidified excess silicon melt in upper strata, open valve 20, open vacuum unit 24, vacuum tightness in graphite bend pipe and graphite guide tube 18 is evacuated to 500Pa, between graphite bend pipe and graphite guide tube and vacuum chamber 2, mineralization pressure is poor, the not solidified excess silicon melt in upper strata enters graphite bend pipe under pressure difference effect, and enter in cold-crucible under the guiding of graphite guide tube 18.
The 3rd step aftertreatment: treat that the not solidified excess silicon melt in upper strata all enters cold-crucible, cut off the electricity supply, stop heating, the tailing that is rich in impurity has just been collected among cold-crucible, after melting finishes, opens collection case lid, reclaim tailing, in crucible, solidifying the ingot casting obtaining is HIGH-PURITY SILICON ingot casting, and its purity will reach 99.999%, and yield rate reaches 95%.
Claims (10)
1. a method for directional freeze tailing quick collection purifying polycrystalline silicon, is characterized in that: in protection of inert gas environment, clean silicon material is heated to melt completely after forming silicon melt is incubated; Lower the temperature afterwards, draw ingot vertically downward, carry out directional freeze; When having solidified 85～90%, stop drawing ingot, graphite bend pipe is stretched in the not solidified excess silicon melt in upper strata, afterwards with vacuum unit to graphite bend pipe the other end extracting vacuum, the not solidified excess silicon melt in upper strata enters in graphite bend pipe under pressure difference effect, and under the guiding of graphite guide tube, enters among water-cooled collection box; Until upper strata, not solidified excess silicon melt all imports after water-cooled collection box, cuts off the electricity supply, and stops heating, in water-cooled collection box, solidify obtain for tailing, in crucible, solidify the ingot casting obtaining and be HIGH-PURITY SILICON ingot casting.
2. the method for a kind of directional freeze tailing quick collection purifying polycrystalline silicon according to claim 1, is characterized in that: the concrete steps of the method that adopts are as follows:
The first step pre-treatment: add the clean silicon material of crucible volume 90～95% in crucible (7), close vent line (13), open vacuum pump group (14), first the vacuum tightness in vacuum chamber (2) is extracted into 0.01-10Pa, close afterwards vacuum pump group, open vent line (13), in vacuum chamber (2), be filled with rare gas element, reach 500～10000Pa to pressure, close vent line (13);
Second step melting, solidify: power-on, utilize ruhmkorff coil (5) and graphite heater (6) that the silicon material in crucible (7) is heated to 1450～1650 ℃ to being fused into silicon melt completely, and be incubated 30～60min at this temperature, pull vertically downward aqueous cold plate (12), make silicon melt in crucible (7) with the speed of 0.1-2mm/min uniform motion vertically downward, draw ingot, silicon melt carries out directional freeze by crucible (7) bottom to top, when silicon melt is solidified to 85～90%, stop drawing ingot, graphite bend pipe (1) is moved down, its lower end extend in the not solidified excess silicon melt in upper strata, open valve (20), open vacuum unit (24), vacuum tightness in graphite bend pipe and graphite guide tube (18) is evacuated to 1-500Pa, between graphite bend pipe and graphite guide tube and vacuum chamber (2), mineralization pressure is poor, the not solidified excess silicon melt in upper strata enters graphite bend pipe under pressure difference effect, and enter in cold-crucible under the guiding of graphite guide tube (18).
The 3rd step aftertreatment: treat that the not solidified excess silicon melt in upper strata all enters cold-crucible, cut off the electricity supply, stop heating, the tailing that is rich in impurity has just been collected among cold-crucible, after melting finishes, opens collection case lid, reclaim tailing, in crucible, solidifying the ingot casting obtaining is HIGH-PURITY SILICON ingot casting, and its purity will reach 99.99%-99.999%, and yield rate reaches 85-95%.
3. according to the method for the arbitrary described a kind of directional freeze tailing quick collection purifying polycrystalline silicon of claim 1 or 2, it is characterized in that: described silicon material is industrial silicon, its purity is 99.0%～99.9%.
4. according to the method for the arbitrary described a kind of directional freeze tailing quick collection purifying polycrystalline silicon of claim 1 or 2, it is characterized in that: described rare gas element is argon gas or helium, its purity is more than 99.9%.
5. the equipment that the method for a kind of directional freeze tailing quick collection purifying polycrystalline silicon according to claim 1 adopts, by vacuum chamber (2), form outer wall, vacuum-lines (15) is installed on outer wall, vacuum-lines (15) one end is connected with vacuum pump group (14), it is characterized in that: on outer wall, be installed with vent line (13), aqueous cold plate (12) is movably installed in vacuum chamber (2) bottom, graphite cake (11) is placed in aqueous cold plate top, graphite cake has hole on (11), graphite pillar (10) one end is 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 on crucible periphery and is fixed on vacuum chamber (2) sidewall, carbon felt insulated tank (4) is placed on outside graphite heater (6) and is fixed on vacuum chamber (2) sidewall, on carbon felt insulation cover (3), have hole, be placed in carbon felt insulated tank (4) top, ruhmkorff coil (5) is placed on outside carbon felt insulated tank (4), and be fixed on vacuum chamber (2) sidewall, graphite bend pipe (1) upper end is fixedly installed on expansion link (22), and its lower end is placed in central position directly over crucible through carbon felt insulation cover (3), graphite bend pipe (1) upper end open place is tightly connected by junctor (19) and graphite guide tube (18) intermediate openings, graphite guide tube upper end air-tight movable is installed on vacuum chamber (2) top, its upper end open is tightly connected by valve (20) and vacuum withdraw device, water-cooled collection box (17) sealing is fixedly installed on vacuum chamber (2) sidewall, graphite bend pipe (1) lower ending opening is connected with water-cooled collection box (17) air-tight movable.
6. the equipment that the method for a kind of directional freeze tailing quick collection purifying polycrystalline silicon according to claim 5 adopts, is characterized in that: at least 3, the hole on described graphite cake (11), graphite pallet has draw-in groove on (9).
7. the equipment that the method for a kind of directional freeze tailing quick collection purifying polycrystalline silicon according to claim 5 adopts, is characterized in that: described graphite bend pipe (1) is sharp mouth graphite bend pipe, and its lower end mouth of pipe is sharp mouth taper.
8. the equipment that the method for a kind of directional freeze tailing quick collection purifying polycrystalline silicon according to claim 5 adopts, is characterized in that: described graphite guide tube (18) middle part is installed with expansion link (22).
9. the equipment that the method for a kind of directional freeze tailing quick collection purifying polycrystalline silicon according to claim 5 adopts, is characterized in that: on described water-cooled collection box (17) outer side wall, be provided with and collect case lid (16)
10. the equipment that the method for a kind of directional freeze tailing quick collection purifying polycrystalline silicon according to claim 5 adopts, it is characterized in that: described vacuum withdraw device adopts bleed line (21) air-tight movable to be installed on graphite guide tube upper end open, vacuum unit (24) is fixedly installed in the other end of bleed line (21), and vacuumometer (23) is installed on bleed line.
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| CN103278351A (en) * | 2013-06-06 | 2013-09-04 | 青岛隆盛晶硅科技有限公司 | Sampling device for silicon melt in medium smelting, and application method thereof |
| CN103498194B (en) * | 2013-09-26 | 2016-01-13 | 青岛隆盛晶硅科技有限公司 | A kind of apparatus for directional solidification and prepare the method for polysilicon |
| CN104860316B (en) * | 2015-05-15 | 2017-06-27 | 大连理工大学 | A kind of electron beam solidification crucible and the method for excluding metal impurities |
| US10918970B2 (en) | 2015-12-30 | 2021-02-16 | Corner Star Limited | Systems and methods for extracting liquid |
| CN110697720B (en) * | 2019-11-19 | 2022-12-09 | 云南永昌硅业股份有限公司 | Device for large industrial silicon rapid directional solidification |
| CN112538653A (en) * | 2020-12-08 | 2021-03-23 | 江苏神汇新材料科技有限公司 | Method for online cleaning of impurity bottom material in single crystal furnace |
| CN114457408A (en) * | 2020-12-08 | 2022-05-10 | 江苏神汇新材料科技有限公司 | Preparation method of gettering tank for cleaning impurity bottom materials in single crystal furnace |
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| CN101913606A (en) * | 2010-08-02 | 2010-12-15 | 大连理工大学 | Composite type heating method and device for polycrystalline silicon smelting |
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| CN102219219A (en) * | 2011-05-16 | 2011-10-19 | 大连隆田科技有限公司 | Method and equipment for purifying polycrystalline silicon by directional solidification and filter slag melting |
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| CN101913606A (en) * | 2010-08-02 | 2010-12-15 | 大连理工大学 | Composite type heating method and device for polycrystalline silicon smelting |
| 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 |
| CN102219219A (en) * | 2011-05-16 | 2011-10-19 | 大连隆田科技有限公司 | Method and equipment for purifying polycrystalline silicon by directional solidification and filter slag melting |
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