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CN108560047A - A kind of heterogeneous nucleation high-efficiency polycrystalline ingot casting crucible processing method - Google Patents

A kind of heterogeneous nucleation high-efficiency polycrystalline ingot casting crucible processing method Download PDF

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Publication number
CN108560047A
CN108560047A CN201810559486.0A CN201810559486A CN108560047A CN 108560047 A CN108560047 A CN 108560047A CN 201810559486 A CN201810559486 A CN 201810559486A CN 108560047 A CN108560047 A CN 108560047A
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CN
China
Prior art keywords
silicon nitride
silicon
silica flour
intermixture
nucleating agent
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Pending
Application number
CN201810559486.0A
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Chinese (zh)
Inventor
郭宽新
刘郭军
方圆
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Henan Shengda Photovoltaic Technology Co Ltd
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Henan Shengda Photovoltaic Technology Co Ltd
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Priority to CN201810559486.0A priority Critical patent/CN108560047A/en
Publication of CN108560047A publication Critical patent/CN108560047A/en
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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B28/00Production of homogeneous polycrystalline material with defined structure
    • C30B28/04Production of homogeneous polycrystalline material with defined structure from liquids
    • C30B28/06Production of homogeneous polycrystalline material with defined structure from liquids by normal freezing or freezing under temperature gradient
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02Elements
    • C30B29/06Silicon

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Silicon Compounds (AREA)

Abstract

The invention is related to a kind of heterogeneous nucleation high-efficiency polycrystalline ingot casting crucible processing method, it includes carborundum powder, silica flour and silicon nitride powder, the treating method comprises following steps:1)By carborundum powder, silica flour, silicon nitride powder, alcohol and pure water mixture, uniform intermixture is stirred into, intermixture is sprayed on to the silica crucible bottom normally sprayed, feeds after nucleating agent drying, throws polycrystalline silicon ingot or purifying furnace ingot casting;2)To ensure the purity of silicon ingot and normally spraying, carborundum powder, silica flour and silicon nitride powder purity in above-mentioned nucleating agent>99.9%, grain size is located at 1~100um;3)Silicon carbide, silica flour and silicon nitride in above-mentioned nucleating agent are mixed into nucleating agent according to a certain percentage;4)After above-mentioned intermixture spraying is dry, deposit thickness is located at 0.1~5mm;5)Above-mentioned intermixture is to spray to the crucible bottom handled well;Therefore, the present invention has the advantages that easy to operate, of low cost, high yield rate, easy to spread.

Description

A kind of heterogeneous nucleation high-efficiency polycrystalline ingot casting crucible processing method
Technical field
The invention belongs to photovoltaic technology field, and in particular to a kind of heterogeneous nucleation high-efficiency polycrystalline ingot casting crucible processing method.
Background technology
It peters out in fossil energy, today of environment worsening, solar power generation becomes human future alternative energy source Hope.Crystal-silicon solar cell is a kind of most advantageous device of solar generating by its high efficiency and high stability, Middle polycrystal silicon cell with higher cost performance, become occupied on Vehicles Collected from Market 80% or more share.But solar battery technology Also immature, photoelectric conversion efficiency is relatively low, cost of electricity-generating is higher etc., and short slabs constrain solar cell large-scale promotion application.Cause This, it is current photovoltaic industry urgent problem to be solved to improve cell photoelectric transfer efficiency and reduce battery manufacture cost.
Polycrystalline silicon solar cell is made in polysilicon chip substrate, and polysilicon crystal defect seriously reduces solar cell Transfer efficiency.The method that silicon ingot for cutting polysilicon chip mainly uses directional solidification is made, this method crystal growing process Control coarse, silicon ingot volume is big, causes silicon ingot built-in thermal stress larger.When thermal stress is more than the shear strength of crystal, stress is just It is discharged in a manner of forming crystal defect.Casting refinement silicon ingot crystal grain, increases grain boundary density, the thermal stress of silicon ingot is made to pass through crystal boundary It is released, the generation of crystal defect can be reduced, to improve battery conversion efficiency.
Existing certain methods at present, as 102826737 A of patent CN provide a kind of quartzy earthenware that bottom roughnessization is handled Crucible promotes crystal nucleation, crystal grain thinning using coarse crucible bottom surface.But the crucible spraying silicon nitride of roughening treatment applies After layer, what is directly contacted with silicon liquid is silicon nitride coating, due to silicon nitride coating and being not wetted by property of silicon liquid, cannot play forming core The effect at center, thus, this method is undesirable to grain morphology improvement.A kind of use that 102776557 A of patent CN are proposed Broken silicon material is layered on crucible bottom and promotes forming core, silicon material to melt the later stage as seed crystal, and adjusting process keeps broken silicon material partial melting, brilliant Body is grown up using not melting silicon material as seed crystal, obtains the silicon ingot of high quality.But the silicon that this method is not melted since bottom has Material, silicon ingot percentage of admixture is higher, and the yield rate of ingot casting is low, and in addition this method needs to accurately control seed crystal surplus, can not also at present Realization automatically controls, and can only manually be detected with quartz pushrod, and the control of seed crystal surplus is unstable, is difficult to realize and popularizes in an all-round way;Cause This, a kind of easy to operate, of low cost, high yield rate of exploitation, heterogeneous nucleation high-efficiency polycrystalline ingot casting crucible easy to spread processing Method has a very important significance.
Invention content
The purpose of the invention is to overcome the deficiencies in the prior art, and provide at a kind of efficient ingot casting crucible of heterogeneous nucleation Reason method, this method are mainly characterized by spraying one layer of non-silicon matter in crucible bottom, reduce surface crystallization energy, start to tie in silicon liquid When brilliant, a large amount of nucleus is formed on bottom, and highdensity crystal boundary reduces the defect concentrations in crystals in polysilicon, improves battery conversion Efficiency, while this method is easy to operate, of low cost, high yield rate, easy to spread.
The object of the present invention is achieved like this:A kind of heterogeneous nucleation high-efficiency polycrystalline ingot casting crucible processing method, it includes Carborundum powder, silica flour and silicon nitride powder, the treating method comprises following steps:
1)By carborundum powder, silica flour, silicon nitride powder, alcohol and pure water mixture, uniform intermixture is stirred into, intermixture is sprayed It is coated in the silica crucible bottom normally sprayed, feeds after nucleating agent drying, throws polycrystalline silicon ingot or purifying furnace ingot casting.
2)To ensure the purity of silicon ingot and normally spraying, the carborundum powder, silica flour and silicon nitride powder in above-mentioned nucleating agent are pure Degree>99.9%, grain size is located at 1~100um.
3)Silicon carbide, silica flour and silicon nitride in above-mentioned nucleating agent are mixed into nucleating agent according to a certain percentage.
4)After above-mentioned intermixture spraying is dry, deposit thickness is located at 0.1~5mm.
5)Above-mentioned intermixture is to spray to the crucible bottom handled well.
The silicon liquid is nucleating center in mixing dose form face, and great number of grains is formed at long brilliant initial stage.
It is more than 99.9% silicon carbide, silica flour and silicon nitride powder using purity, silica flour and silicon nitride grain size are less than 100um, press According to weight ratio 30%:20%:50% mixing takes weight 300g, is dissolved in the prepared solvents of 300mL, is configured to intermixture.
Silicon carbide in the above-mentioned nucleating agent, ratio range is 10%~40% in silica flour, silicon nitride powder:5%~40%: 20%~85%.
The dosage of the above-mentioned nucleating agent is:It is sprayed on crucible after drying, is 0.1mm in the deposition thickness of crucible ~3mm.
The ratio of the pure water mixture and alcohol is 100:1 to 3:Between 1.
Beneficial effects of the present invention:Several nucleating agents of the present invention are easy to get, and method is simple, easy to operate;It is cast using the present invention Ingot, silicon chip crystal defect is less, minority carrier life time higher, and more conventional polysilicon chip battery efficiency improves 0.3~0.5%;Use this hair Bright ingot casting, silicon ingot yield rate, ingot casting cost are suitable with conventional foundry ingot;Easy to operate using ingot casting of the present invention, properties of product are steady It is fixed, it is not required to increase equipment, is easy to a large amount of Rapid Popularizations;Therefore, the present invention have easy to operate, of low cost, high yield rate, easily In promote the advantages of.
Specific implementation mode
Embodiment 1
1)Using purity more than 99.9%, silicon carbide, silica flour and silicon nitride powder, silica flour and silicon nitride grain size are less than 100um, press According to weight ratio 30%:20%:50% mixing takes weight 300g, is dissolved in the prepared solvents of 300mL, is configured to intermixture.
2)Solvent pure water and alcohol are respectively 270ml and 30ml.
3)Crucible internal walls are according to common process spraying silicon nitride coating, mixed in the spraying of crucible bottom half after coating drying Mixture.
4)Crucible temperature is kept to be completely dried for 20-100 DEG C to intermixture, deposit thickness about 0.1~0.3mm.
5)According to the charging of conventional foundry ingot technique, ingot casting.
6)It takes with and without the spraying small side's ingot in intermixture part, comparison grain morphology, corrosion default, test minority carrier life time are simultaneously received Whole silicon chips are taken to carry out battery efficiency comparison.
Comparing result is as follows:
By comparison, evenly, corrosion default density is lower for spraying intermixture part silicon ingot crystal grain smaller, silicon ingot minority carrier life time compared with Without the high 0.4us in intermixture part, spraying intermixture part average cell efficiency is high by 0.32% compared with no intermixture part, and efficiency Distribution more restrains.
Embodiment 2
A kind of heterogeneous nucleation high-efficiency polycrystalline ingot casting crucible processing method, it includes carborundum powder, silica flour and silicon nitride powder, the place Reason method includes the following steps:
1)By carborundum powder, silica flour, silicon nitride powder, alcohol and pure water mixture, uniform intermixture is stirred into, intermixture is sprayed It is coated in the silica crucible bottom normally sprayed, feeds after nucleating agent drying, throws polycrystalline silicon ingot or purifying furnace ingot casting.
2)To ensure the purity of silicon ingot and normally spraying, the carborundum powder, silica flour and silicon nitride powder in above-mentioned nucleating agent are pure Degree>99.9%, grain size is located at 1~100um.
3)Silicon carbide, silica flour and silicon nitride in above-mentioned nucleating agent are mixed into nucleating agent according to a certain percentage.
4)After above-mentioned intermixture spraying is dry, deposit thickness is located at 0.1~5mm.
5)Above-mentioned intermixture is to spray to the crucible bottom handled well;The silicon liquid is forming core in mixing dose form face Center forms great number of grains at long brilliant initial stage;It is more than 99.9% silicon carbide, silica flour and silicon nitride powder, silica flour and nitrogen using purity SiClx grain size is less than 100um, according to weight ratio 30%:20%:50% mixing takes weight 300g, is dissolved in the prepared solvents of 300mL In, it is configured to intermixture;Silicon carbide in the above-mentioned nucleating agent, ratio range is 10%~40% in silica flour, silicon nitride powder:5% ~40%:20%~85%;The dosage of the above-mentioned nucleating agent is:It is sprayed on crucible after drying, is in the deposition thickness of crucible 0.1mm~3mm;The ratio of the pure water mixture and alcohol is 100:1 to 3:Between 1.
Specific implementation mode is unrestricted to further explanation of the invention, is existed for those of ordinary skills Further transformation is done to structure in the case of not departing from substantive content of the present invention, and all these transformation should all belong to institute of the present invention Attached scope of the claims.

Claims (6)

1. a kind of heterogeneous nucleation high-efficiency polycrystalline ingot casting crucible processing method, it includes carborundum powder, silica flour and silicon nitride powder, spy Sign is:It the treating method comprises following steps:
1)By carborundum powder, silica flour, silicon nitride powder, alcohol and pure water mixture, uniform intermixture is stirred into, intermixture is sprayed It is coated in the silica crucible bottom normally sprayed, feeds after nucleating agent drying, throws polycrystalline silicon ingot or purifying furnace ingot casting.
2)To ensure the purity of silicon ingot and normally spraying, carborundum powder, silica flour and silicon nitride powder purity in above-mentioned nucleating agent> 99.9%, grain size is located at 1~100um.
3)Silicon carbide, silica flour and silicon nitride in above-mentioned nucleating agent are mixed into nucleating agent according to a certain percentage.
4)After above-mentioned intermixture spraying is dry, deposit thickness is located at 0.1~5mm.
5)Above-mentioned intermixture is to spray to the crucible bottom handled well.
2. a kind of heterogeneous nucleation high-efficiency polycrystalline ingot casting crucible processing method according to claim 1, it is characterised in that:It is described Silicon liquid is nucleating center in mixing dose form face, and great number of grains is formed at long brilliant initial stage.
3. a kind of heterogeneous nucleation high-efficiency polycrystalline ingot casting crucible processing method according to claim 1, it is characterised in that:It uses Purity is more than 99.9% silicon carbide, silica flour and silicon nitride powder, and silica flour and silicon nitride grain size are less than 100um, according to weight ratio 30%: 20%:50% mixing takes weight 300g, is dissolved in the prepared solvents of 300mL, is configured to intermixture.
4. a kind of heterogeneous nucleation high-efficiency polycrystalline ingot casting crucible processing method according to claim 1, it is characterised in that:It is described Silicon carbide in above-mentioned nucleating agent, ratio range is 10%~40% in silica flour, silicon nitride powder:5%~40%:20%~85%.
5. a kind of heterogeneous nucleation high-efficiency polycrystalline ingot casting crucible processing method according to claim 1, it is characterised in that:Institute The dosage for stating above-mentioned nucleating agent is:It is sprayed on crucible after drying, is 0.1mm~3mm in the deposition thickness of crucible.
6. a kind of heterogeneous nucleation high-efficiency polycrystalline ingot casting crucible processing method according to claim 1, it is characterised in that:It is described The ratio of pure water mixture and alcohol is 100:1 to 3:Between 1.
CN201810559486.0A 2018-06-02 2018-06-02 A kind of heterogeneous nucleation high-efficiency polycrystalline ingot casting crucible processing method Pending CN108560047A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109913929A (en) * 2019-04-29 2019-06-21 常州大学 A kind of novel ingot casting crucible pad pasting and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104195632A (en) * 2014-09-04 2014-12-10 奥特斯维能源(太仓)有限公司 Method for casting high efficiency polycrystalline silicon ingots
US20150056123A1 (en) * 2012-04-01 2015-02-26 Jiang Xi Sai Wei Ldk Solar Hi-Tech Co., Ltd. Polycrystalline silicon ingot, preparation method thereof, and polycrystalline silicon wafer
CN104532344A (en) * 2014-12-09 2015-04-22 烟台同立高科新材料股份有限公司 Preparation method of efficient silicon nitride powder for polycrystalline silicon ingots

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20150056123A1 (en) * 2012-04-01 2015-02-26 Jiang Xi Sai Wei Ldk Solar Hi-Tech Co., Ltd. Polycrystalline silicon ingot, preparation method thereof, and polycrystalline silicon wafer
CN104195632A (en) * 2014-09-04 2014-12-10 奥特斯维能源(太仓)有限公司 Method for casting high efficiency polycrystalline silicon ingots
CN104532344A (en) * 2014-12-09 2015-04-22 烟台同立高科新材料股份有限公司 Preparation method of efficient silicon nitride powder for polycrystalline silicon ingots

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109913929A (en) * 2019-04-29 2019-06-21 常州大学 A kind of novel ingot casting crucible pad pasting and preparation method thereof

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Application publication date: 20180921