CN104711673A - Preparation method of polycrystalline silicon ingot - Google Patents
Preparation method of polycrystalline silicon ingot Download PDFInfo
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- CN104711673A CN104711673A CN201510112780.3A CN201510112780A CN104711673A CN 104711673 A CN104711673 A CN 104711673A CN 201510112780 A CN201510112780 A CN 201510112780A CN 104711673 A CN104711673 A CN 104711673A
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Abstract
The invention relates to a preparation method of a polycrystalline silicon ingot. The method comprises the following steps: (1) a binding agent, a dispersing agent, and silicon particles of which the purity is above 99.9 percent and the diameter is between 1 [mu]m and 5,000 [mu]m, are added into deionized water, a pulp is obtained after uniform mixing, and the mass percentage of the silicon particles in the pulp is not less than 50 percent; (2) in a quartz crucible with a silicon nitride coating on the inner surface, the pulp is applied on the surface of the silicon nitride coating through spray coating, roller coating or brush coating, so as to form a pulp layer with a thickness between 1 mm and 10 mm; the crucible with a silicon coating is obtained after drying; (3) the crucible with the silicon coating is sent into a polycrystalline silicon ingot furnace after being loaded with silicon materials, the silicon materials are heated after vacuum pumping, a silicon material melt is cooled for polycrystalline silicon growth after the silicon materials are completely molten, and the polycrystalline silicon ingot is obtained through annealing cooling after the polycrystalline silicon growth is completed. The polycrystalline silicon ingot obtained through the method can be used for the manufacturing of a solar battery, so that the average battery efficiency of a silicon wafer exceeds 18 percent.
Description
Technical field
The present invention relates to a kind of preparation method of polycrystalline silicon ingot casting.
Background technology
In photovoltaic field, crystalline silicon, due to its raw material sources and preparation cost advantage, accounts for more than 90% of whole photovoltaic field.And in the preparation process of crystalline silicon, take status as the leading factor with polycrystalline silicon ingot casting technology again.At present, existing polysilicon foundry engieering mainly contains fine melt efficient polycrystalline silicon ingot casting technology and has seed crystal ingot casting technology (including accurate monocrystalline ingot casting and fritting high-efficiency polycrystalline ingot casting technology more popular at present).
The key distinction of this several crystalline silicon ingot casting technology is, accurate monocrystalline ingot casting and fritting high-efficiency polycrystalline ingot casting must be equipped with seed crystal in crucible bottom at when filling with substance, also can be described as seed crystal ingot casting technology, and need ensure that this seed crystal is not completely melted in later stage melting process, using the nucleating center as later stage crystal growth, otherwise just become common polycrystalline ingot casting.The special seeding layer that fine melt efficient polycrystalline silicon ingot casting technology makes with crucible bottom, for medium, utilizes the roughness of crucible bottom to promote the forming core that ingot casting is initial, the good polysilicon of growth quality.In this ingot casting technology, silicon material melts completely, and need need not protect seed crystal as having seed crystal ingot casting technology, therefore can continue to use thermal field and the technique of conventional polysilicon ingot casting completely, and can obtain the higher-quality polycrystal silicon ingot of more traditional common polycrystalline.
The patent No. is CN103014852 A, name of patent application is a kind of method for casting efficient polycrystalline silicon ingot, provide a kind of mixture spraying silica flour and pure water on quartz crucible silicon nitride coating, the crack between the silica flour coating of utilization be full of cracks is as the method for forming core point growing polycrystalline silicon ingot.This method making processes is unstable, and belongs to the one of fine melt efficient polycrystalline silicon ingot casting technology, does not have with the advantage of silicon class material for forming core point growing polycrystalline silicon ingot.
Summary of the invention
The technical problem that the present invention solves by providing nucleus growth point for polycrystalline silicon growth, has higher photoelectric transformation efficiency after making the polysilicon of formation make solar cell, the polycrystalline silicon ingot casting stable performance of making.
Technical scheme of the present invention is, a kind of preparation method of polycrystalline silicon ingot casting is provided, comprise the following steps: (1) adds the silicon grain that binding agent, dispersion agent and purity are greater than 99.9%, particle diameter is 1 ~ 5000 μm in deionized water, stir and obtain slurry, the mass percent that wherein silicon grain accounts for slurry is not less than 50%; (2) be provided with in the quartz crucible of silicon nitride coating at internal surface, by described slurry spraying, roller coat or brushing on silicon nitride coating surface, form the pulp layer of 1 ~ 10mm, drying obtains silicon coating crucible; (3) described silicon coating crucible is loaded onto silicon material, send into polycrystalline silicon ingot or purifying furnace, after vacuumizing, to the heating of silicon material, after silicon material all melts, silicon material liquation is lowered the temperature and carries out polycrystalline silicon growth, after polycrystalline silicon growth completes, obtain polycrystalline silicon ingot casting through annealing cooling.
Further, in described step (1), also add in deionized water purity more than 99.99%, particle diameter is 0.1 ~ 10 μm of silicon nitride powder, the mass percent that wherein silicon nitride powder accounts for slurry is no more than 20%.
Further, the purity of described silicon grain is greater than 99.999%, and particle diameter is 100 ~ 500 μm.
Further, described binding agent is selected from one or more in silicon sol, silicic acid, polyvinyl alcohol and acrylate.
Further, described dispersion agent is selected from one or more in unit alcohol, polyvalent alcohol, methylcellulose gum, ethyl cellulose, rhodia, propyl cellulose and polyethylene oxide.
Further, in described step (3), before described silicon coating crucible is loaded onto silicon material, first lay polycrysalline silcon or fragment in silicon coating crucible bottom.
The detailed step of technical scheme of the present invention is as follows: (i) gets out the crucible of a polycrystalline silicon ingot casting, often selects quartz crucible, carries out the making of conventional nitridation silicon coating to quartz crucible; (ii) in deionized water, add binding agent, dispersion agent and silicon grain, mixing and stirring obtains slurry, and silicon grain chooses the silicon grain of purity more than 99.9%, and preferably, the purity of silicon grain is more than 99.999%, and particle diameter is 100 ~ 500 μm; (iii) slurry is covered on silicon nitride coating in the mode such as spraying, roller coat or brushing, form the pulp layer of one deck 1 ~ 10mm, adopt and to dry or the mode such as oven dry carries out drying treatment, obtain silicon coating crucible; (iv) silicon raw material and electroactive adulterant are loaded silicon coating crucible, the electroactive adulterant of use is used for adjusting the resistivity of silicon ingot; Preferably, electroactive adulterant uses borosilicate alloy, and target resistivity is set to 0.8 ~ 3 Ω cm; V the crucible installing silicon material is put into ingot furnace by (), vacuumize and heat, and after the fusing of silicon material, the silicon material of crucible bottom molten state for the quick forming core crystallization of seed crystal, forms forming core active layer with the silicon grain in pulp layer.Crystalline silicon completes directional solidification growth from the bottom up, generates polycrystal silicon ingot.Can first lay polycrysalline silcon or fragment in crucible bottom in step (iv), play the effect of protective paste layer.Can use fine melt thermal field and technique in step (v), the present invention is comparatively loose to the temperature control requirement at crystal growth initial stage, and process window is larger; Also can use fritting thermal field and technique, reduce fritting leapfrog height, even if seed crystalization is complete or fractionated complete, the silicon grain in pulp layer also can be utilized to be seed crystal, generate high-quality casting polycrystalline silicon ingot.
In step (ii), except adding binding agent in deionized water, outside dispersion agent and silicon grain, also add purity more than 99.99%, particle diameter is 0.1 ~ 10 μm of silicon nitride powder, the mass percent that wherein silicon nitride powder accounts for slurry is no more than 20%.Because silicon nitride powder is comparatively thin, can be filled in the gap of silicon grain, can particulate material be protected and not easily melt; In addition, it is tightr that the silicon nitride powder added can be combined with the silicon nitride coating of bottom, also contributes to supercoat and do not come off.
The preparation method of polycrystalline silicon ingot casting disclosed by the invention, combines fine melt efficient polycrystalline silicon ingot casting technology and the advantage having seed crystal ingot casting technology, on the basis that silicon material melts completely, with silicon class material for forming core medium, and growth efficient polycrystalline silicon ingot casting.And adopt the inventive method to casting ingot process require relatively low, have easy to operate, cost is low, cell photoelectric efficiency of conversion advantages of higher.
The preparation method of polycrystalline silicon ingot casting provided by the invention, form one deck pulp layer by covering on the conventional nitridation silicon coating of quartz crucible, crystalline silicon is with the silicon grain in pulp layer for seed crystal realizes directional solidification growth, and the crystalline silicon defect of preparation is few, and quality is high.
The present invention utilizes the method for fine melt polycrystalline silicon ingot casting, prepares the product close with fritting polycrystalline silicon ingot casting quality, has ingot casting and must expect that rate is high, cost is low, battery efficiency high, and simple to operate, is easy to scale operation.
The present invention have easy to operate, cost is low, cell photoelectric efficiency of conversion advantages of higher.The polysilicon adopting the inventive method to prepare has crystal grain and is evenly distributed, dislocation defects is few, the solar cell that polycrystalline silicon ingot casting the present invention obtained is made, battery efficiency is higher by 0.4% ~ 1% than common polycrystalline silicon solar cell efficiency, and average cell efficiency is more than 18%.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1:
A preparation method for polycrystalline silicon ingot casting provided by the invention, concrete steps are as follows, use G5 type ingot furnace to carry out ingot casting, select G5 quartz crucible, carry out the making of conventional nitridation silicon coating to crucible.Select the silicon grain material of purity more than 99.999%, particle diameter is 200 ~ 400 μm, and weight is 1kg; In deionized water, add silicon sol, polyvinyl alcohol and alcohol, obtain solution after mixing, the quality of solution is 0.2kg; Silicon grain and solution are mixed and obtains slurry.The slurry mode of brushing is covered on silicon nitride coating, forms the pulp layer that one deck is about 1mm, dry rear stand-by.Silicon raw material and electroactive adulterant are loaded in silicon coating crucible, gross weight is 500kg, and target resistivity is set to 1.8 Ω cm, then is sent in ingot furnace by silicon coating crucible, vacuumizes rear operation casting ingot process, completes ingot casting process.
The silicon ingot obtained through evolution, check, block, plain grinding, chamfering, the link such as section obtain polysilicon chip.In silicon chip, homogeneous grain size is consistent, and be made into cell piece, record its average efficiency and reach 18.1%, top efficiency reaches 18.85%.
Embodiment 2:
A kind of preparation method of polycrystalline silicon ingot casting provided by the invention, concrete steps are as follows, G5 type ingot furnace is used to carry out ingot casting, select G5 quartz crucible, the making of conventional nitridation silicon coating is carried out to crucible, select the silicon grain material through grinding after of purity more than 99.99%, particle diameter is 1 ~ 100 μm, weight is 5kg, silicon grain material is used hydrogen peroxide cleaning, carries out 80 DEG C of oven dry afterwards.In deionized water, add silicon sol and methylcellulose gum, obtain solution after mixing, the quality of solution is 0.5kg; Silicon grain material and solution are mixed and obtains slurry.Slurry is covered on silicon nitride coating with spraying method, forms the pulp layer that one deck is about 5mm, stand-by after drying.When filling with substance, is laid on crucible bottom by 20kg silicon grain material, then loads in silicon coating crucible by excess silicon raw material and electroactive adulterant, sends in ingot furnace, vacuumize rear operation casting ingot process, complete ingot casting process.
The silicon ingot obtained through evolution, check, block, plain grinding, chamfering, the link such as section obtain polysilicon chip.In silicon chip, homogeneous grain size is consistent, and dislocation defects is less, is made into cell piece, and record its average efficiency and reach 18.05%, top efficiency reaches 18.9%.
Embodiment 3:
A preparation method for polycrystalline silicon ingot casting provided by the invention, concrete steps are as follows, use G6 type ingot furnace to carry out ingot casting, select G6 quartz crucible, carry out the making of conventional nitridation silicon coating to crucible.Select the silicon grain material of purity more than 99.9%, particle diameter is 100 ~ 5000 μm, and weight is 1kg; Select the silicon nitride powder of purity more than 99.99%, particle diameter is 0.1 ~ 1 μm, and weight is 0.1kg; After being mixed with silicon nitride powder by silicon grain, use alcohol-pickled cleaning, carry out 80 DEG C of drying and processings afterwards.In deionized water, add silicon sol and methylcellulose gum, obtain solution after mixing, the quality of solution is 0.2kg; The mixture of silicon grain and silicon nitride powder and solution are mixed and obtains slurry.Slurry is covered on silicon nitride coating with roll coating model, forms the pulp layer that one deck is about 4mm, stand-by after drying.When filling with substance, is laid on crucible bottom by 5kg particulate material, then loads in the quartz crucible after process by excess silicon raw material and electroactive adulterant, sends in ingot furnace, vacuumize rear operation casting ingot process, complete ingot casting process.
The silicon ingot obtained through evolution, check, block, plain grinding, chamfering, the link such as section obtain polysilicon chip.In silicon chip, homogeneous grain size is consistent, and be made into cell piece, record its average efficiency and reach 18.2%, top efficiency reaches 19.1%.
Embodiment 4:
A preparation method for polycrystalline silicon ingot casting provided by the invention, concrete steps are as follows, use G6 type ingot furnace to carry out ingot casting, select G6 quartz crucible, the making of conventional nitridation silicon coating is carried out to crucible, select the silicon grain material of purity more than 99.999%, particle diameter is 100 ~ 5000 μm, and weight is 1kg; Select the silicon nitride powder of purity more than 99.99%, particle diameter is 0.1 ~ 10 μm, and weight is 0.5kg; After being mixed with silicon nitride powder by silicon grain, add silicon sol, acrylate, methylcellulose gum and polyethylene oxide, obtain solution after mixing in deionized water, the quality of solution is 3kg; The mixture of silicon grain and silicon nitride powder and solution are mixed and obtains slurry.Slurry is covered on conventional nitridation silicon coating with spraying method, forms the pulp layer that one deck is about 10mm, stand-by after drying.When filling with substance, silicon raw material and electroactive adulterant are loaded in the quartz crucible after process, gross weight is 800kg, and target resistivity is set to 1.5 Ω cm.Again the quartz crucible that 800kg material is housed is sent in ingot furnace, vacuumize rear operation casting ingot process, complete ingot casting process.
The silicon ingot obtained through evolution, check, block, plain grinding, chamfering, the link such as section obtain polysilicon chip.In silicon chip, homogeneous grain size is consistent, and be made into cell piece, record its average efficiency and reach 18.0%, top efficiency reaches 18.6%.
Embodiment 5:
A preparation method for polycrystalline silicon ingot casting provided by the invention, concrete steps are as follows, use G6 type ingot furnace to carry out ingot casting, select G6 quartz crucible, the making of conventional nitridation silicon coating is carried out to crucible, select the silicon grain material of purity more than 99.999%, particle diameter is 100 ~ 500 μm, and weight is 0.5kg; Select the silicon grain material of purity more than 99.99%, particle diameter is 10 ~ 50 μm, and weight is 0.5kg; After two kinds of silicon grain material mixing, use alcohol-pickled cleaning, carry out 80 DEG C of drying and processings afterwards.In deionized water, add silicon sol and methylcellulose gum, obtain solution after mixing, the quality of solution is 0.1kg; Silicon grain material and solution are mixed and obtains slurry.Slurry is covered on silicon nitride coating in brushing mode, forms the pulp layer that one deck is about 1mm, stand-by after drying.When filling with substance, silicon raw material and electroactive adulterant are loaded in the quartz crucible after process, gross weight is 800kg, and target resistivity is set to 1.5 Ω cm.Again the quartz crucible that 800kg material is housed is sent in ingot furnace, vacuumize rear operation casting ingot process, complete ingot casting process.
The silicon ingot that above-described embodiment is obtained through evolution, check, block, plain grinding, chamfering, the link such as section obtain polysilicon chip.In silicon chip, homogeneous grain size is consistent, and be made into cell piece, record its average light photoelectric transformation efficiency and reach 18.15%, top efficiency reaches 18.78%.
Claims (6)
1. a preparation method for polycrystalline silicon ingot casting, is characterized in that, comprises the following steps:
(1) add the silicon grain that binding agent, dispersion agent and purity are greater than 99.9%, particle diameter is 1 ~ 5000 μm in deionized water, stir and obtain slurry, the mass percent that wherein silicon grain accounts for slurry is not less than 50%;
(2) be provided with in the quartz crucible of silicon nitride coating at internal surface, by described slurry spraying, roller coat or brushing on silicon nitride coating surface, form the pulp layer of 1 ~ 10mm, drying obtains silicon coating crucible;
(3) described silicon coating crucible is loaded onto silicon material, send into polycrystalline silicon ingot or purifying furnace, after vacuumizing, to the heating of silicon material, after silicon material all melts, silicon material liquation is lowered the temperature and carries out polycrystalline silicon growth, after polycrystalline silicon growth completes, obtain polycrystalline silicon ingot casting through annealing cooling.
2. preparation method as claimed in claim 1, it is characterized in that, in described step (1), also add in deionized water purity more than 99.99%, particle diameter is 0.1 ~ 10 μm of silicon nitride powder, the mass percent that wherein silicon nitride powder accounts for slurry is no more than 20%.
3. preparation method as claimed in claim 1 or 2, it is characterized in that, the purity of described silicon grain is greater than 99.999%, and particle diameter is 100 ~ 500 μm.
4. preparation method as claimed in claim 1 or 2, it is characterized in that, described binding agent is selected from one or more in silicon sol, silicic acid, polyvinyl alcohol and acrylate.
5. preparation method as claimed in claim 1 or 2, it is characterized in that, described dispersion agent is selected from one or more in unit alcohol, polyvalent alcohol, methylcellulose gum, ethyl cellulose, rhodia, propyl cellulose and polyethylene oxide.
6. preparation method as claimed in claim 1 or 2, is characterized in that, in described step (3), before described silicon coating crucible is loaded onto silicon material, first lays polycrysalline silcon or fragment in silicon coating crucible bottom.
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| CN105063748A (en) * | 2015-08-14 | 2015-11-18 | 烟台核晶陶瓷新材料有限公司 | Efficient crucible for polycrystal ingot casting and preparation method of efficient crucible |
| CN105177710A (en) * | 2015-10-28 | 2015-12-23 | 镇江环太硅科技有限公司 | Manufacturing method for novel full-melting efficient crucible |
| CN105332049A (en) * | 2015-10-29 | 2016-02-17 | 镇江环太硅科技有限公司 | Preparation method of G6 low-impurity-diffusion low-dislocation-density high-purity efficient crucible |
| CN105780114A (en) * | 2016-05-20 | 2016-07-20 | 江苏协鑫硅材料科技发展有限公司 | Silicon ingot and preparation method thereof |
| CN106747664A (en) * | 2016-11-17 | 2017-05-31 | 苏州阿特斯阳光电力科技有限公司 | The production method of the preparation method, crucible and polysilicon silicon chip of the coating of crucible |
| CN107312432A (en) * | 2017-06-23 | 2017-11-03 | 石家庄优士科电子科技有限公司 | Polycrystalline silicon ingot casting silica crucible silicon nitride coating binding agent and preparation method thereof |
| CN108262237A (en) * | 2018-01-23 | 2018-07-10 | 镇江环太硅科技有限公司 | A kind of efficient G7 crucible coating layers preparation method |
| CN108517557A (en) * | 2018-05-22 | 2018-09-11 | 英利能源（中国）有限公司 | The preparation method and efficient polycrystalline silicon ingot of efficient polycrystalline silicon ingot |
| CN110359090A (en) * | 2019-08-20 | 2019-10-22 | 浙江晶科能源有限公司 | The casting ingot method and crystalline silicon of a kind of ingot casting seed crystal, crystalline silicon |
| CN111733453A (en) * | 2019-03-25 | 2020-10-02 | 中材江苏太阳能新材料有限公司 | Crucible for polycrystalline silicon ingot casting and preparation method thereof |
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| CN108262237A (en) * | 2018-01-23 | 2018-07-10 | 镇江环太硅科技有限公司 | A kind of efficient G7 crucible coating layers preparation method |
| CN108517557A (en) * | 2018-05-22 | 2018-09-11 | 英利能源（中国）有限公司 | The preparation method and efficient polycrystalline silicon ingot of efficient polycrystalline silicon ingot |
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