CN201857440U - Crucible for purification and ingot casting of solar-grade polysilicon - Google Patents
Crucible for purification and ingot casting of solar-grade polysilicon Download PDFInfo
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- CN201857440U CN201857440U CN2010205870291U CN201020587029U CN201857440U CN 201857440 U CN201857440 U CN 201857440U CN 2010205870291 U CN2010205870291 U CN 2010205870291U CN 201020587029 U CN201020587029 U CN 201020587029U CN 201857440 U CN201857440 U CN 201857440U
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Abstract
The utility model discloses a crucible for purification and ingot casting of solar-grade polysilicon, which comprises a crucible body made of quartz materials. A crucible coating which is made from water glass, silicon nitride powder, barium hydroxide powder and nanometer silicon dioxide powder is coated on the inner wall of the crucible body. The crucible can effectively prevent coating particles from peeling to pollute silicon crystals, and simultaneously has impurity removal effect.
Description
Technical field
The utility model relates to a kind of crucible, particularly relates to the crucible that a kind of solar-grade polysilicon purification ingot casting is used.
Background technology
Because Siemens process polycrystalline silicon purification techniques production cost height, and the purity of the silicon of Siemens Method production reaches 11N, and solar energy level silicon only is 6～7N to the requirement of purity, therefore, Siemens Method is applied to the silicon solar cell field of making and will cause unnecessary resource and cost waste.In recent years, adopt the technology of metallurgy method purification preparation solar-grade polysilicon to obtain to pay attention to widely.
The metallurgy method purification techniques need be through the refining and the ingot casting of silicon materials, and the charge cask of employing is generally quartz crucible.Because the fusing point of silicon is higher, refining and ingot casting are consuming time longer, and at high temperature Long contact time unavoidably chemical reaction will take place between silicon liquid and the crucible.On the one hand, reaction can cause oxygen element and other impurity element to dissolve in the silicon liquid, and silicon liquid is polluted, and influences the electric property of silicon crystal.On the other hand, reaction can cause silicon ingot and crucible to stick together, and causes difficulty to the demoulding.And because silicon crystal is different with the thermal expansivity of crucible material, produce stress between the silicon ingot of adhesion and the crucible, cause the generation of lattice defect, even silicon ingot and crucible are cracked.Therefore,, be convenient to the demoulding, and obtain pure, ideal silicon crystal, need at inner wall of quartz crucible spraying one deck supercoat for preventing reaction and the adhesion between ingot casting and the crucible.Have good tack between these protective layer need and the crucible, and high temperature resistant, silicon melt is not polluted.
Usually the main component of the coated material that adopts is a silicon nitride.Crucible is coated with after the last layer silicon nitride coating, can stop the chemical reaction between silicon liquid and the crucible, helps the demoulding, makes the repeated use of quartz crucible become possibility, thereby reduces production costs.Yet the intensity of common silicon nitride coating is not high.Though silicon nitride coating through oversintering, in use easily peels off, silicon nitride particle enters in the silicon melt, be present in the silicon crystal at last, thus defectives such as impurity in the increase silicon crystal and dislocation.
Water glass is often used as the tackiness agent of coating powder, can effective fixed coating powder, prevent coating shedding.But at high temperature, the main component sodium in the water glass can produce crucible material and corrode.
The utility model content
The technical problems to be solved in the utility model provides the crucible that a kind of solar-grade polysilicon purification ingot casting is used.By having applied one deck crucible coating layer in the crucible inner body wall, make this crucible can prevent effectively that coating particles from peeling off and cause the particle contamination silicon crystal, simultaneously owing in coating, add and to suppress sodium under the high temperature to the composition of the destruction of crucible with in refining process, help the composition of removal of impurities, therefore, has impurity-eliminating effect.
For solving the problems of the technologies described above, the crucible that solar-grade polysilicon purification ingot casting of the present utility model is used, the crucible body that comprises quartzy material, wherein, to have applied one deck be the crucible coating layer that raw material is made by water glass, alpha-silicon nitride powders, hydrated barta powder and nano-silica powder end to the inwall of this crucible body.
The thickness of described crucible coating layer is 30～300 microns.
Wherein, the preparation method of described crucible coating layer comprises step:
(1) making of water glass
With high-purity sodium carbonate and glass sand with weight ratio be mix at 1: 1.5 after, after 1400～1600 ℃ of fusions, the deionized water of flowing through obtains fusion water glass particle, by 120～160 ℃ water vapor, heats after 4～5 hours again, obtains water glass;
(2) water glass, alpha-silicon nitride powders, hydrated barta powder and nano-silica powder end are mixed after, be coated on the crucible inner body wall after, oven drying at low temperature; Wherein, water glass: the weight ratio of total weight of solids is 1: 0.8～1: 1.2, and total weight of solids is three's weight sum of silicon nitride, hydrated barta and nano silicon;
(3) the crucible body after the oven dry enters process furnace, after 1～8 hour, obtains one deck fine and close uniformly supercoat in the crucible inner body wall in 800～1000 ℃ of sintering.
The purity of the high-purity sodium carbonate in the described step (1) is more than 99.9%; The purity of high purity quartz is more than 99.99%, and wherein boron, phosphorus content are lower than 0.1ppm; The granularity of high-purity sodium carbonate and high purity quartz is less than 200 orders.
Silicon nitride in the described step (2) and hydrated barta powder size are between 1000～2000 orders, and silicon nitride and hydrated barta purity all are more than 99.9%, and silicon nitride is 5: 1～20: 1 with the mixed weight ratio of hydrated barta powder.The granularity at nano-silica powder end is 20～50nm, and the purity at nano-silica powder end is more than 99.99%, and wherein boron, phosphorus content less than 0.1ppm; The add-on at nano-silica powder end accounts for 5～25% of total weight of solids, and wherein, total weight of solids is three's weight sum of silicon nitride, hydrated barta and nano silicon.
Coating method in the described step (2) is spraying or brushing; The crucible body is the quartz crucible body.
Oven drying at low temperature in the described step (3) is under 60～100 ℃, dries 1～8 hour.
By adopting solvent and the binding agent of water glass as silicon nitride, when sintering, sodium in the water glass and moisture content and carbonic acid gas all volatilize, silicon nitride can with the silicon oxide crucibles mortise, silicon nitride particle is solidificated on the crucible inwall, thereby can prevent that silicon nitride particle from peeling off, destroy the growth of silicon crystal, pollute silicon crystal.The adding of nano silicon can suppress under the high temperature sodium to the destruction of quartz crucible, and improves the bonding strength between coating and the matrix and the smooth finish of coating.Add hydrated barta in crucible coating layer, high temperature reacts with silicon and boron impurities wherein down, and generation BOH gas volatilizees with SiO, thereby can play the effect except that boron.
Adopt the crucible coating layer of method for preparing, obtain polysilicon behind the refining ingot casting, adopt SEM (scanning electron microscope) to analyze to its crystal growth situation, find that crystal growth is complete, grain-size is thick, no particle contamination situation.
Adopt ICP-MS (plasma mass spectrograph) to carry out content analysis, the boron content of handling in the silicon of back is boron content low 10～20% in the silicon that obtains than the general silicon nitride coating crucible of employing.
Description of drawings
Below in conjunction with accompanying drawing and embodiment the utility model is described in further detail:
Accompanying drawing is a crucible structural representation of the present utility model, and 1 is crucible coating layer, and 2 is the crucible body.
Embodiment
In following examples, high-purity sodium carbonate of employing, high purity quartz, silicon nitride, hydrated barta, nano silicon all are the commercially available prod, and wherein, the purity of high-purity sodium carbonate is 99.98%; The purity of high purity quartz is 99.99%, and wherein boron, phosphorus content are lower than 0.1ppm; The granularity of high-purity sodium carbonate and high purity quartz is less than 200 orders; The purity of silicon nitride is more than 99.9%; The purity of hydrated barta is 99.9%; The purity of nano silicon is 99.999%, and wherein boron, phosphorus content less than 0.1ppm; Silicon nitride and hydrated barta powder size are between 1000～2000 orders; The granularity at nano-silica powder end is 20～50nm.
In addition, in following examples, polysilicon that obtains behind the refining ingot casting and utilization are coated with the silicon that crucible obtains, and all are to operate according to a conventional method.
The crucible that solar-grade polysilicon purification ingot casting is used, its structural representation is shown in Figure of description, the crucible body 2 that comprises quartzy material, wherein, to have applied one deck be the crucible coating layer 1 that raw material is made by water glass, alpha-silicon nitride powders, hydrated barta powder and nano-silica powder end to the inwall of crucible body 2.The thickness of this crucible coating layer 1 is 30～300 microns.
Wherein, crucible coating layer 1 is a solar-grade polysilicon purification crucible for casting ingots coating 1, and the preparation method of this crucible coating layer 1 comprises step:
(1) making of water glass
Is mixing in 1: 1.5 with high-purity sodium carbonate and glass sand with weight ratio, and after 1500 ℃ of fusions, the deionized water of flowing through obtains fusion water glass particle; By 140 ℃ water vapor, heat 5 hours preparation water glass again.
(2) be mixing in 5: 1 by weight with alpha-silicon nitride powders and hydrated barta powder; add 5% nano silicon [be nano silicon account for total weight of solids 5%; wherein; total weight of solids is a silicon nitride; three's weight sum of hydrated barta and nano silicon]; with the solid state powder (silicon nitride that mixes; three's sum of hydrated barta and nano silicon) be after 1: 1 mixed is mixed well by weight with water glass; spray to quartz crucible body 2 inwalls; after drying 6 hours under 60 ℃; 900 ℃ of following sintering 6 hours, obtain the fine and close supercoat uniformly of one deck at crucible body 2 inwalls at last.
Adopt the crucible coating layer 1 of present embodiment preparation, obtain polysilicon behind the refining ingot casting, adopt SEM (scanning electron microscope) to analyze, find that crystal growth is complete, crystal grain radial dimension average out to 9.7mm, no particle contamination situation its crystal growth situation.Adopt ICP-MS (plasma mass spectrograph) to carry out content analysis, the boron content of handling in the silicon of back is boron content low 16% in the silicon that obtains than the general silicon nitride coating crucible of employing.
The crucible that solar-grade polysilicon purification ingot casting in the present embodiment is used is as embodiment 1, but wherein, the preparation method of crucible coating layer 1 is as follows:
(1) making of water glass
Is mixing in 1: 1.5 with high-purity sodium carbonate and glass sand with weight ratio, and after 1400 ℃ of fusions, the deionized water of flowing through obtains fusion water glass particle; By 120 ℃ water vapor, heat 4.5 hours preparation water glass again.
(2) be mixing in 10: 1 by weight with alpha-silicon nitride powders and hydrated barta powder; the nano silicon of adding 10%; after the mixed that the solid state powder that mixes and water glass are 1: 1 is by weight mixed well; brush quartz crucible body 2 inwalls; dried 1 hour down at 100 ℃; 1000 ℃ of following sintering 1 hour, obtain the fine and close supercoat uniformly of one deck at crucible body 2 inwalls at last at last.
Adopt the crucible coating layer 1 of present embodiment preparation, obtain polysilicon behind the refining ingot casting, adopt SEM (scanning electron microscope) to analyze, find that crystal growth is complete, crystal grain radial dimension average out to 10.2mm, no particle contamination situation its crystal growth situation.Adopt ICP-MS (plasma mass spectrograph) to carry out content analysis, the boron content of handling in the silicon of back is boron content low 13% in the silicon that obtains than the general silicon nitride coating crucible of employing.
Embodiment 3
The crucible that solar-grade polysilicon purification ingot casting in the present embodiment is used is as embodiment 1, but wherein, the preparation method of crucible coating layer 1 is as follows:
(1) making of water glass
Is mixing in 1: 1.5 with high-purity sodium carbonate and glass sand with weight ratio, and after 1600 ℃ of fusions, the deionized water of flowing through obtains fusion water glass particle; By 160 ℃ water vapor, heat 4 hours preparation water glass again.
(2) be mixing in 15: 1 by weight with alpha-silicon nitride powders and hydrated barta powder; the nano-silica powder end of adding 15%; after the mixed that the solid state powder that mixes and water glass are 1: 1 is by weight mixed well; spray to quartz crucible body 2 inwalls; dried 3 hours down at 80 ℃; 800 ℃ of following sintering 3 hours, obtain the fine and close supercoat uniformly of one deck at crucible body 2 inwalls at last at last.
Adopt the crucible coating layer 1 of present embodiment preparation, obtain polysilicon behind the refining ingot casting, adopt SEM (scanning electron microscope) to analyze, find that crystal growth is complete, crystal grain radial dimension average out to 12.5mm, no particle contamination situation its crystal growth situation.Adopt ICP-MS (plasma mass spectrograph) to carry out content analysis, the boron content of handling in the silicon of back is boron content low 15% in the silicon that obtains than the general silicon nitride coating crucible of employing.
Embodiment 4
The crucible that solar-grade polysilicon purification ingot casting in the present embodiment is used is as embodiment 1, but wherein, the preparation method of crucible coating layer 1 is as follows:
(1) making of water glass
Is mixing in 1: 1.5 with high-purity sodium carbonate and glass sand with weight ratio, and after 1450 ℃ of fusions, the deionized water of flowing through obtains fusion water glass particle; By 150 ℃ water vapor, heat 4 hours preparation water glass again.
(2) be mixing in 20: 1 by weight with alpha-silicon nitride powders and hydrated barta powder; the nano-silica powder end of adding 25%; the mixed that the solid state powder that mixes and water glass are 1: 1 is by weight mixed well; brush quartz crucible body 2 inwalls; dried 8 hours down at 70 ℃; 1000 ℃ of following sintering 8 hours, obtain the fine and close supercoat uniformly of one deck at crucible body 2 inwalls at last at last.
Adopt the crucible coating layer 1 of present embodiment preparation, obtain polysilicon behind the refining ingot casting, adopt SEM (scanning electron microscope) to analyze, find that crystal growth is complete, crystal grain radial dimension average out to 12.8mm, no particle contamination situation its crystal growth situation.Adopt ICP-MS (plasma mass spectrograph) to carry out content analysis, the boron content of handling in the silicon of back is boron content low 18% in the silicon that obtains than the general silicon nitride coating crucible of employing.
Embodiment 5
The crucible that solar-grade polysilicon purification ingot casting in the present embodiment is used is as embodiment 1, but wherein, the preparation method of crucible coating layer 1 is as follows:
(1) making of water glass
Is mixing in 1: 1.5 with high-purity sodium carbonate and glass sand with weight ratio, and after 1550 ℃ of fusions, the deionized water of flowing through obtains fusion water glass particle; By 130 ℃ water vapor, heat 4.2 hours preparation water glass again.
(2) be mixing in 8: 1 by weight with alpha-silicon nitride powders and hydrated barta powder; the nano-silica powder end of adding 20%; the mixed that the solid state powder that mixes and water glass are 1: 0.8 is by weight mixed well; brush quartz crucible body 2 inwalls; dried 5 hours down at 90 ℃; 850 ℃ of following sintering 5 hours, obtain the fine and close supercoat uniformly of one deck at crucible body 2 inwalls at last at last.
Adopt the crucible coating layer 1 of present embodiment preparation, obtain polysilicon behind the refining ingot casting, adopt SEM (scanning electron microscope) to analyze, find that crystal growth is complete, crystal grain radial dimension average out to 11.2mm, no particle contamination situation its crystal growth situation.Adopt ICP-MS (plasma mass spectrograph) to carry out content analysis, the boron content of handling in the silicon of back is boron content low 12% in the silicon that obtains than the general silicon nitride coating crucible of employing.
Embodiment 6
The crucible that solar-grade polysilicon purification ingot casting in the present embodiment is used is as embodiment 1, but wherein, the preparation method of crucible coating layer 1 is as follows:
(1) making of water glass
Is mixing in 1: 1.5 with high-purity sodium carbonate and glass sand with weight ratio, and after 1580 ℃ of fusions, the deionized water of flowing through obtains fusion water glass particle; By 1450 ℃ water vapor, heat 4.8 hours preparation water glass again.
(2) be mixing in 12: 1 by weight with alpha-silicon nitride powders and hydrated barta powder; the nano-silica powder end of adding 12%; the mixed that the solid state powder that mixes and water glass are 1: 1.2 is by weight mixed well; spray to quartz crucible body 2 inwalls; dried 4 hours down at 65 ℃; 950 ℃ of following sintering 4 hours, obtain the fine and close supercoat uniformly of one deck at crucible body 2 inwalls at last at last.
Adopt the crucible coating layer 1 of present embodiment preparation, obtain polysilicon behind the refining ingot casting, adopt SEM (scanning electron microscope) to analyze, find that crystal growth is complete, crystal grain radial dimension average out to 12.3mm, no particle contamination situation its crystal growth situation.Adopt ICP-MS (plasma mass spectrograph) to carry out content analysis, the boron content of handling in the silicon of back is boron content low 18% in the silicon that obtains than the general silicon nitride coating crucible of employing.
Claims (2)
1. crucible that solar-grade polysilicon purification ingot casting is used, this crucible comprises the crucible body of quartzy material, it is characterized in that: the inwall of described crucible body has applied one deck crucible coating layer.
2. the crucible that solar-grade polysilicon purification ingot casting as claimed in claim 1 is used is characterized in that: the thickness of described crucible coating layer is 30～300 microns.
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| CN103088417A (en) * | 2013-01-22 | 2013-05-08 | 晶海洋半导体材料（东海）有限公司 | High-efficiency crucible for polycrystal ingot casting and preparation method thereof |
| CN103320854A (en) * | 2013-06-07 | 2013-09-25 | 英利集团有限公司 | Coating structure for crucible, preparation method thereof, and crucible with coating structure |
| CN103435370A (en) * | 2013-08-09 | 2013-12-11 | 天津大学 | High-binding-strength silicon nitride coating of quartz ceramic crucible prepared through co-sintering method |
| CN103827351A (en) * | 2011-08-31 | 2014-05-28 | Esk陶瓷有限及两合公司 | Silicon-nitride-containing interlayer of great hardness |
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| CN103827351A (en) * | 2011-08-31 | 2014-05-28 | Esk陶瓷有限及两合公司 | Silicon-nitride-containing interlayer of great hardness |
| US9625213B2 (en) | 2011-08-31 | 2017-04-18 | 3M Innovative Properties Company | Silicon-nitride-containing separating layer having high hardness |
| CN104583464A (en) * | 2012-06-25 | 2015-04-29 | 希利柯尔材料股份有限公司 | Lining for surfaces of a refractory crucible for purification of silicon and method of purification of the silicon melt using that crucible (s) for melting and further directional solidification |
| CN103088417A (en) * | 2013-01-22 | 2013-05-08 | 晶海洋半导体材料（东海）有限公司 | High-efficiency crucible for polycrystal ingot casting and preparation method thereof |
| CN103088417B (en) * | 2013-01-22 | 2016-08-03 | 晶海洋半导体材料（东海）有限公司 | A kind of polycrystalline cast ingot high efficient crucible and preparation method thereof |
| CN103320854A (en) * | 2013-06-07 | 2013-09-25 | 英利集团有限公司 | Coating structure for crucible, preparation method thereof, and crucible with coating structure |
| CN103320854B (en) * | 2013-06-07 | 2016-03-02 | 英利集团有限公司 | Crucible coating structure, its preparation method and comprise its crucible |
| CN103435370A (en) * | 2013-08-09 | 2013-12-11 | 天津大学 | High-binding-strength silicon nitride coating of quartz ceramic crucible prepared through co-sintering method |
| CN106801252A (en) * | 2016-12-30 | 2017-06-06 | 江西中材太阳能新材料有限公司 | A kind of quartz ceramic crucible for polycrystalline silicon ingot casting and preparation method thereof |
| CN106801252B (en) * | 2016-12-30 | 2019-06-18 | 江西中材太阳能新材料有限公司 | A kind of quartz ceramic crucible for polycrystalline silicon ingot casting and preparation method thereof |
| CN108560046A (en) * | 2018-04-19 | 2018-09-21 | 常熟华融太阳能新型材料有限公司 | It is a kind of improve polycrystalline silicon ingot casting crystalline substance flower silicon nitride exempt from spray-on coating and preparation method thereof |
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Assignee: Jiangsu strong Photovoltaic Technology Co., Ltd. Assignor: Shanghai Pro Entergy Technology Co., Ltd. Contract record no.: 2012320000363 Denomination of utility model: Crucible for purification and ingot casting of solar-grade polysilicon Granted publication date: 20110608 License type: Exclusive License Record date: 20120330 |
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Granted publication date: 20110608 Termination date: 20131102 |