CN104805499A - N type polycrystalline ingot casting equipment and process for preparing N type polycrystalline ingot - Google Patents
N type polycrystalline ingot casting equipment and process for preparing N type polycrystalline ingot Download PDFInfo
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- CN104805499A CN104805499A CN201510252512.1A CN201510252512A CN104805499A CN 104805499 A CN104805499 A CN 104805499A CN 201510252512 A CN201510252512 A CN 201510252512A CN 104805499 A CN104805499 A CN 104805499A
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Abstract
The invention provides N type polycrystalline ingot casting equipment and a process for preparing an N type polycrystalline ingot. According to the N type polycrystalline ingot casting equipment, an improvement, namely additionally arranging a set of secondary feeding devices, is made on original equipment for preparing a P type polycrystalline cast ingot, so that the N type polycrystalline ingot can be cast, no equipment needs to be changed, and thus the production cost is reduced. By the adoption of the process disclosed by the invention, the electrical resistivity of the N type polycrystalline ingot prepared by adopting the equipment provided by the invention is more uniform, and the homogeneity of a battery piece is improved.
Description
Technical field
The present invention relates to a kind of N-type polycrystalline cast ingot equipment and preparation technology thereof, belong to polycrystalline silicon ingot casting technical field.
Background technology
Along with the sustainable development of photovoltaic industry, the technique of cell piece obtains rapid progress, wherein N-type battery slice technique is considered as following high point of strategy by each large enterprises especially, relative P type battery, N-type battery slice its have higher efficiency of conversion, the unit surface generated energy of photovoltaic module can be driven further, and installation cost.And the segregation coefficient of the doping agent phosphorus element of N-type silicon chip is relatively low, and as the polycrystalline cast ingot process program that main flow P-type silicon sheet supplies, the qualified silicon rod of sufficiently long resistivity can not be obtained, the extremely low cost that causes of yield rate is high, N-type polycrystalline silicon sheet can not be provided according to the technology mode of original production P-type silicon sheet, this will cause a large amount of production capacity wastes, delays industry progress.
The problem bringing again metal by adding gallium as the scheme that counter doping agent makes up yield rate of Zhejiang University's invention, and the silicon material of end segment will unconditionally be scrapped, cost is drawn high.
Summary of the invention
The present invention proposes a kind of N-type polycrystalline cast ingot equipment and preparation technology thereof, can solve the problem.
For realizing this purpose, the method applied in the present invention is: a kind of N-type polycrystalline cast ingot equipment, comprise upper cavity and lower chamber, described upper cavity covers on lower chamber, it is seal cup bottom described lower chamber, lower warming plate is set above seal cup, quartz crucible is provided with in described upper cavity, it is heat exchange mass bottom quartz crucible, above quartz crucible, well heater is set, described upper cavity top arranges a secondary charging device, described secondary charging device comprises storage bin and feeding storehouse, storage bin is positioned at above feeding storehouse, plate is provided with between two feed bins, plate controls folding by push-pull valve, described storage bin top is provided with charging opening cover plate, charging opening cover plate is provided with the second viewing window, feeding tube is connected bottom described feeding storehouse, feeding tube leads to quartz crucible, manual rotation baffle plate is provided with between described feeding storehouse and feeding tube, heat insulation plate is provided with below manual rotation baffle plate, folding is controlled by heat insulation push-pull valve.
Be provided with crucible in described feeding storehouse, what crucible adopted is special-shaped centrum high purity quartz.
Described upper cavity top is provided with explosion relief valve and the first viewing window, and explosion relief valve connects well heater.
Lifting rotation mechanism is provided with between described storage bin and feeding storehouse.
Hard carbon felt is enclosed with outside described feeding storehouse, preliminary heating zone is provided with outside hard carbon felt, copper electrode is provided with in described preliminary heating zone, insulated column is enclosed with bottom copper electrode, quartz ring is wrapped up outside described preliminary heating zone, be provided with intermediate layer of water-flowing outside quartz ring, feeding storehouse connect gas ducting and vacuum lead, and thermopair is set.
Tubular zirconium-oxide is enclosed with outside described feeding tube.
Utilize equipment described in claim 1 to prepare a technique for N-type polycrystalline silicon ingot, first melt part silicon material and carry out crystal growth, then progressively add silicon material, described technique concrete steps are as follows:
(1) in quartz crucible, load 500kg original silicon material and N-type mother alloy in advance, after batching, phosphorus content controls to 45.3ppba;
(2) well heater is opened, and is melted by the silicon material in quartz crucible, then carries out crystal growth, controls crystal growth rate and is less than 1.5cm/h, and slow down gradually to 1.1cm/h;
(3) the silicon material in storage bin and doping agent are dropped in feeding storehouse by criticizing, be evacuated to-600bar by feeding storehouse and storage bin, open preliminary heating zone and make temperature progressively be warming up to 1000 DEG C, in storehouse, be filled with argon gas simultaneously remove air, 10-50kg is a collection of, carries out in batches;
(4), when the growing height of crystal is to 18cm in calculating quartz crucible, suspends and automatically control, change Non-follow control and carry out intensification 5-10 DEG C, reduce heat-insulation cage position 1-3cm;
(5) heat insulation push-pull valve is first opened, open manual rotation baffle plate again, the granular polycrystalline silicon being preheated to 1000 DEG C is sent in quartz crucible, mix with the silicon material in former quartz crucible, change the concentration of impurities in silicon material in quartz crucible, manual rotation baffle plate is first closed after feeding, close heat insulation push-pull valve again, continue to carry out preheating by storage bin feeding to feeding storehouse, preheating temperature to when 1000 DEG C again feeding enter in body of heater, preheating silicon material and feeding enter in the process in body of heater, push-pull valve and manual rotation baffle plate can not be opened simultaneously, cyclic preheat and feeding enter stove till this reinforced 150kg,
(6), during temperature before the temperature recovery in quartz crucible to secondary charging, recover to perform temperature and control, recover heat-insulation cage position, proceed crystal growth, growth velocity is 1.1cm/h simultaneously;
(7), when calculating growing height to 30-32cm, running (3), (5) step is repeated, this reinforced 120kg;
(8) after temperature index is replied, silicon ingot grows complete by Controlling Growth Rate 1.1cm/h, and after crystal growth end signal provides, go to annealing and process for cooling, wait is come out of the stove.
Its beneficial effect is: this equipment improves on the equipment of original preparation P type polycrystalline silicon ingot casting, add a set of secondary charging device, N-type polycrystalline silicon ingot can be cast, without the need to more exchange device, reduce production cost, adopt technique of the present invention more even by the resistivity of the N-type polycrystalline silicon ingot obtained by equipment of the present invention, improve the uniformity of cell piece.
Accompanying drawing explanation
Fig. 1 is casting unit structural representation of the present invention;
Fig. 2 is secondary charging device structural representation of the present invention.
Embodiment
All features disclosed in this specification sheets, or the step in disclosed all methods or process, except mutually exclusive feature and/or step, all can combine by any way.
Arbitrary feature disclosed in this specification sheets (comprising any accessory claim, summary and accompanying drawing), unless specifically stated otherwise, all can be replaced by other equivalences or the alternative features with similar object.That is, unless specifically stated otherwise, each feature is an example in a series of equivalence or similar characteristics.
A kind of N-type polycrystalline cast ingot equipment as shown in Figure 1, comprise upper cavity 2 and lower chamber 1, described upper cavity 2 covers on lower chamber 1, is seal cup 3, arranges lower warming plate 4 above seal cup 3 bottom described lower chamber 1.Be provided with quartz crucible 5 in upper cavity 2, be heat exchange mass 6 bottom quartz crucible 5, well heater 9 is set above quartz crucible 5, in well heater 9, be provided with temperature-detecting device.Upper cavity 2 top is provided with explosion relief valve 8 and the first viewing window 7, and explosion relief valve 8 connects well heater 9, prevents quartz crucible 5 internal pressure excessive.
Upper cavity 2 top arranges a secondary charging device 10, secondary charging device 10 as shown in Figure 2, comprise storage bin 101 and feeding storehouse 102, storage bin 101 is positioned at above feeding storehouse 2, be provided with plate between two feed bins, plate controls folding by push-pull valve 105, is provided with lifting rotation mechanism 106 between storage bin 101 and feeding storehouse 102, storage bin can be carried out rotation and lifting, facilitate the maintenance of storage bin and feeding storehouse.Described storage bin 101 top is provided with charging opening cover plate 103, and charging opening cover plate 103 is provided with the second viewing window 104.
Be provided with crucible in feeding storehouse 102, what crucible adopted is special-shaped centrum high purity quartz, prevents the container of other materials from producing silicon material and pollutes.Connect feeding tube 1019 bottom described feeding storehouse 102, feeding tube 1019 leads to quartz crucible 5, is enclosed with tubular zirconium-oxide 1018 outside feeding tube 1019.Be enclosed with hard carbon felt 1012 outside the crucible of feeding storehouse 102, outside hard carbon felt 1012, be provided with preliminary heating zone 1010.Be provided with copper electrode 1014 in described preliminary heating zone 1010, copper electrode 1014 is safeguarded by high purity graphite, is connected, heats crucible by graphite with copper electrode 1014 with transformer.Insulated column 1013 is enclosed with bottom copper electrode 1014.Wrap up quartz ring 109 outside described preliminary heating zone 1010, quartz ring can play fixed action to the crucible of inside, prevents crucible from breaking.Be provided with intermediate layer of water-flowing 1011 outside quartz ring 109, intermediate layer of water-flowing 1011 is cooled feeding storehouse by cooling circulating water.Feeding storehouse 102 connects gas ducting 107 and vacuum lead 108, and thermopair 1016 is set.Vacuum lead 108 pairs of storage bins and feeding storehouse vacuumize, and prevent outside air to the pollution of silicon material, and gas ducting 107 carry rare gas element argon gas in storehouse, can play uniform heat-field, the effect of pressurize and isolated air.Thermopair 1016 connects temperature control unit, can carry out temperature detection monitoring to feeding storehouse 102.Be provided with manual rotation baffle plate 1015 between feeding storehouse 102 and feeding tube 1019, below manual rotation baffle plate 1015, be provided with heat insulation plate, control folding by heat insulation push-pull valve 1017.
Utilize aforesaid device to carry out the preparation of N polycrystal silicon ingot, its processing step is:
(1) in quartz crucible, load 500kg original silicon material and N-type mother alloy in advance, after batching, phosphorus content controls to 45.3ppba;
(2) well heater is opened, and is melted by the silicon material in quartz crucible, then carries out crystal growth, controls crystal growth rate and is less than 1.5cm/h, and slow down gradually to 1.1cm/h;
(3) the silicon material in storage bin and doping agent are dropped in feeding storehouse by criticizing, be evacuated to-600bar by feeding storehouse and storage bin, open preliminary heating zone and make temperature progressively be warming up to 1000 DEG C, in storehouse, be filled with argon gas simultaneously remove air, 10-50kg is a collection of, carries out in batches;
(4), when the growing height of crystal is to 18cm in calculating quartz crucible, suspends and automatically control, change Non-follow control and carry out intensification 5-10 DEG C, reduce heat-insulation cage position 1-3cm;
(5) heat insulation push-pull valve is first opened, open manual rotation baffle plate again, the granular polycrystalline silicon being preheated to 1000 DEG C is sent in quartz crucible, mix with the silicon material in former quartz crucible, change the concentration of impurities in silicon material in quartz crucible, manual rotation baffle plate is first closed after feeding, close heat insulation push-pull valve again, continue to carry out preheating by storage bin feeding to feeding storehouse, preheating temperature to when 1000 DEG C again feeding enter in body of heater, preheating silicon material and feeding enter in the process in body of heater, push-pull valve and manual rotation baffle plate can not be opened simultaneously, cyclic preheat and feeding enter stove till this reinforced 150kg,
(6), during temperature before the temperature recovery in quartz crucible to secondary charging, recover to perform temperature and control, recover heat-insulation cage position, proceed crystal growth, growth velocity is 1.1cm/h simultaneously;
(7), when calculating growing height to 30-32cm, running (3), (5) step is repeated, this reinforced 120kg;
(8) after temperature index is replied, silicon ingot grows complete by Controlling Growth Rate 1.1cm/h, and after crystal growth end signal provides, go to annealing and process for cooling, wait is come out of the stove.
Utilize the P-type silicon ingot that equipment and process of the present invention grows, crystal weight is compared original casting ingot process section and is promoted 8%-40%, improves productive rate.And its resistivity of N-type silicon ingot utilizing technique of the present invention to grow is more even, the N-type crystal length that can realize more than 80% meets the performance requriements of N-type cell, compares traditional technology yield rate higher, for N-type 6-3 ohmcm, yield rate reaches 70%, and traditional technology only has 49%.Equipment proposed by the invention, without the need to manufacturing brand-new equipment, only need be transformed, reduce production cost, avoid scrapping of large number quipments on the basis of original polycrystalline ingot furnace.
The basis of technique of the present invention can also add automatic feeding system, grow continuously to realize continuous charging, the resistivity that the N-type obtained is specified is more even, improves the uniformity of cell piece further.
The present invention is not limited to aforesaid embodiment.The present invention expands to any new feature of disclosing in this manual or any combination newly, and the step of the arbitrary new method disclosed or process or any combination newly.
Claims (7)
1. a N-type polycrystalline cast ingot equipment, comprise upper cavity (2) and lower chamber (1), it is characterized in that, described upper cavity (2) covers on lower chamber (1), described lower chamber (1) bottom is seal cup (3), seal cup (3) top arranges lower warming plate (4), quartz crucible (5) is provided with in described upper cavity (2), quartz crucible (5) bottom is heat exchange mass (6), quartz crucible (5) top arranges well heater (9), described upper cavity (2) top arranges a secondary charging device (10), described secondary charging device (10) comprises storage bin (101) and feeding storehouse (102), storage bin (101) is positioned at feeding storehouse (2) top, plate is provided with between two feed bins, plate controls folding by push-pull valve (105), described storage bin (101) top is provided with charging opening cover plate (103), charging opening cover plate (103) is provided with the second viewing window (104), described feeding storehouse (102) bottom connects feeding tube (1019), feeding tube (1019) leads to quartz crucible (5), manual rotation baffle plate (1015) is provided with between described feeding storehouse (102) and feeding tube (1019), manual rotation baffle plate (1015) below is provided with heat insulation plate, folding is controlled by heat insulation push-pull valve (1017).
2. N-type polycrystalline cast ingot equipment according to claim 1, is characterized in that, described feeding storehouse is provided with crucible in (102), and what crucible adopted is special-shaped centrum high purity quartz.
3. N-type polycrystalline cast ingot equipment according to claim 1, it is characterized in that, described upper cavity (2) top is provided with explosion relief valve (8) and the first viewing window (7), and explosion relief valve (8) connects well heater (9).
4. N-type polycrystalline cast ingot equipment according to claim 1, is characterized in that, is provided with lifting rotation mechanism (106) between described storage bin (101) and feeding storehouse (102).
5. N-type polycrystalline cast ingot equipment according to claim 1, it is characterized in that, described feeding storehouse (102) outside is enclosed with hard carbon felt (1012), hard carbon felt (1012) outside is provided with preliminary heating zone (1010), copper electrode (1014) is provided with in described preliminary heating zone (1010), copper electrode (1014) bottom is enclosed with insulated column (1013), described preliminary heating zone (1010) outside parcel quartz ring (109), quartz ring (109) outside is provided with intermediate layer of water-flowing (1011), feeding storehouse (102) connects gas ducting (107) and vacuum lead (108), and thermopair (1016) is set.
6. N-type polycrystalline cast ingot equipment according to claim 5, is characterized in that, described feeding tube (1019) outside is enclosed with tubular zirconium-oxide (1018).
7. utilize equipment described in claim 1 to prepare a technique for N-type polycrystalline silicon ingot, it is characterized in that, first melt part silicon material and carry out crystal growth, then progressively add silicon material, described technique concrete steps are as follows:
(1) in quartz crucible, load 500kg original silicon material and N-type mother alloy in advance, after batching, phosphorus content controls to 45.3ppba;
(2) well heater is opened, and is melted by the silicon material in quartz crucible, then carries out crystal growth, controls crystal growth rate and is less than 1.5cm/h, and slow down gradually to 1.1cm/h;
(3) the silicon material in storage bin and doping agent are dropped in feeding storehouse by criticizing, be evacuated to-600bar by feeding storehouse and storage bin, open preliminary heating zone and make temperature progressively be warming up to 1000 DEG C, in storehouse, be filled with argon gas simultaneously remove air, 10-50kg is a collection of, carries out in batches;
(4), when the growing height of crystal is to 18cm in calculating quartz crucible, suspends and automatically control, change Non-follow control and carry out intensification 5-10 DEG C, reduce heat-insulation cage position 1-3cm;
(5) heat insulation push-pull valve is first opened, open manual rotation baffle plate again, the granular polycrystalline silicon being preheated to 1000 DEG C is sent in quartz crucible, mix with the silicon material in former quartz crucible, change the concentration of impurities in silicon material in quartz crucible, manual rotation baffle plate is first closed after feeding, close heat insulation push-pull valve again, continue to carry out preheating by storage bin feeding to feeding storehouse, preheating temperature to when 1000 DEG C again feeding enter in body of heater, preheating silicon material and feeding enter in the process in body of heater, push-pull valve and manual rotation baffle plate can not be opened simultaneously, cyclic preheat and feeding enter stove till this reinforced 150kg,
(6), during temperature before the temperature recovery in quartz crucible to secondary charging, recover to perform temperature and control, recover heat-insulation cage position, proceed crystal growth, growth velocity is 1.1cm/h simultaneously;
(7), when calculating growing height to 30-32cm, running (3), (5) step is repeated, this reinforced 120kg;
(8) after temperature index is replied, silicon ingot grows complete by Controlling Growth Rate 1.1cm/h, and after crystal growth end signal provides, go to annealing and process for cooling, wait is come out of the stove.
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| CN108914200A (en) * | 2018-07-28 | 2018-11-30 | 上海怡英新材料科技有限公司 | A kind of crystal growth system |
| CN113882015A (en) * | 2021-09-29 | 2022-01-04 | 西安奕斯伟材料科技有限公司 | Nitrogen-doped agent feeding device and method and manufacturing system of nitrogen-doped silicon single crystal rod |
| CN114959875A (en) * | 2021-02-26 | 2022-08-30 | 晶科能源股份有限公司 | Feeding equipment for crystal growth device, crystal growth device and feeding process |
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