CN102877129B - A kind of crystalline silicon and preparation method thereof - Google Patents
A kind of crystalline silicon and preparation method thereof Download PDFInfo
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- CN102877129B CN102877129B CN201210333308.9A CN201210333308A CN102877129B CN 102877129 B CN102877129 B CN 102877129B CN 201210333308 A CN201210333308 A CN 201210333308A CN 102877129 B CN102877129 B CN 102877129B
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Abstract
The invention discloses a kind of preparation method of crystalline silicon, comprise the following steps: lay seed of single crystal silicon at random at crucible bottom center, form inculating crystal layer, forming core source is laid at all the other positions, bottom, forms forming core active layer; Inculating crystal layer and forming core active layer arrange the silicon material of molten state, controls crucible bottom temperature and inculating crystal layer and forming core active layer are not completely melted; Temperature in control crucible, along vertical and the described crucible bottom direction gradient of rising formation temperature gradually upwards, makes the silicon material forming core crystallization on seed of single crystal silicon and forming core source after melting, and formation center is the peripheral crystalline silicon for high-efficiency polycrystalline of class monocrystalline.The invention also discloses the crystalline silicon obtained by above-mentioned preparation method.Preparation method of the present invention decreases the consumption of seed of single crystal silicon, saves production cost, improves the quality of the region silico briquette near crucible wall; In the obtained same silicon ingot of crystalline silicon, existing class silicon single crystal has efficient polycrystalline silicon again, achieves the mutual supplement with each other's advantages of class monocrystalline and high-efficiency polycrystalline.
Description
Technical field
The present invention relates to semi-conductor preparation field, especially a kind of crystalline silicon simultaneously containing class monocrystalline and high-efficiency polycrystalline and preparation method thereof.
Background technology
Crystalline silicon uses semiconductor material the most general in solar cell manufacture, and the crystalline silicon at present for the manufacture of solar cell mainly adopts the silicon single crystal of vertical pulling method and adopts the polysilicon of ingot casting technology.Polycrystalline silicon ingot casting, charging capacity is large, simple to operate, process costs is low, but battery conversion efficiency is low, the life-span is short; Pulling of silicon single crystal efficiency of conversion is high, but single feeds intake few, and complicated operation, cost is high.How both united two into one, form mutual supplement with each other's advantages, become focus and the difficult point of current solar photovoltaic industry development.Under this background, the class monocrystalline between polysilicon and silicon single crystal has progressed into the visual field of people.
Class monocrystalline (Mono Like), also known as the monocrystalline that is as the criterion, is the technique based on polycrystalline cast ingot, and in long brilliant process, use single crystal seed by part, acquisition outward appearance and electrical property are all similar to the polysilicon chip of monocrystalline.Class monocrystalline silicon piece to the efficiency of conversion of sun power far above polysilicon, silicon single crystal even shoulder to shoulder, but its manufacturing process and polysilicon similar, the significantly low and silicon single crystal of manufacturing cost, thus becomes rapidly the manufacturing new lover of solar cell.
But, the production of current class monocrystalline silicon piece there is no ripe technique, generally first be paved with seed of single crystal silicon (as Fig. 1) in crucible bottom in prior art, and then fill silicon material, control crucible bottom temperature through heating and melting seed crystal is not melted completely, making silicon liquid not grown by the seed crystal that melts completely, growing the class monocrystalline with single crystal structure.The consumption of this technique not only seed crystal is large, and manufacturing cost is high, and due to the homogeneity of thermal field and directional property, be difficult to grow monocrystalline near the region of crucible wall, most of region is polycrystalline (as Fig. 2), has had a strong impact on the ratio of monocrystalline.Because this region is the region that monocrystalline and polycrystalline coexist, crystal grain extrudes mutually, and dislocation is very easily expanded and bred, and cause the silico briquette in this region of poor quality, battery conversion efficiency is low, even lower than common polycrystalline silicon chip.
Summary of the invention
In order to solve the problems of the technologies described above, the invention provides a kind of preparation method of crystalline silicon, the consumption of the method not only seed crystal reduces further, and greatly improves the quality of the region silico briquette near crucible wall.The present invention also also discloses the crystalline silicon obtained by this preparation method.
First aspect, the invention provides a kind of preparation method of crystalline silicon, comprises the following steps:
(1) lay seed of single crystal silicon at random at crucible bottom center, form inculating crystal layer, the crystal orientation of described seed of single crystal silicon is not limit; Forming core source is laid at all the other positions, bottom, forms forming core active layer;
(2) the silicon material of molten state is set on described inculating crystal layer and forming core active layer, control described crucible bottom temperature lower than described seed crystal and forming core source fusing point, described inculating crystal layer and forming core active layer are not completely melted;
(3) temperature in described crucible is controlled along vertical with the described crucible bottom direction gradient of rising formation temperature gradually upwards, make the silicon material forming core crystallization on described seed of single crystal silicon and forming core source after melting, formation center is the peripheral crystalline silicon for high-efficiency polycrystalline of class monocrystalline;
Preferably, the seed of single crystal silicon described in step (1) is square or circular arrangement at crucible bottom center, close contact between seed of single crystal silicon and seed crystal.
Preferably, the thickness of the inculating crystal layer described in step (1) is 5 ~ 50mm.
Preferably, described in step (1), the particle diameter in forming core source is 0.1um ~ 1cm.
Preferably, described in step (1), the thickness of forming core active layer is 1 ~ 30mm.
Preferably, forming core source described in step (1) is selected from silica flour, the silicon based compound close with the lattice of silicon material and react one or more in the material generating silicon based compound with silicon material, or silica flour, and the close silicon based compound of the lattice of silicon material and react the mixture of one or more and silicon nitride in the material generating silicon based compound with silicon material.
More preferably, the described silicon based compound close with the lattice of silicon material is carborundum powder or silica powder.
It is more preferably, described that to react with silicon material the material generating silicon based compound be carbon dust.
Preferably, the silicon material arranging molten state in step (2) on described inculating crystal layer and forming core active layer is: loading solid silicon material above described inculating crystal layer and forming core active layer, carrying out heating to described crucible makes described silicon material melting form silicon liquid, now, the silicon material of described molten state is arranged at the surface of described inculating crystal layer and forming core active layer.Also preferably, the silicon material arranging molten state in step (2) on described inculating crystal layer and forming core active layer is: heat solid silicon material in another one crucible, the silicon material of obtained molten state, be equipped with in the crucible of forming core active layer described in the silicon material of described molten state is poured into, now, the silicon material of described molten state is arranged at the surface of described inculating crystal layer and forming core active layer.
In step (2), the silicon material being arranged on the molten state on forming core active layer surface has sub-fraction to drop onto in the gap in forming core source, and rapid nucleation under exceeding cold state, obtain based on the small grains in crystal orientation, (110) (112).
Inculating crystal layer described in step (2) and forming core active layer are not completely melted and refer to part inculating crystal layer and the fusing of forming core active layer, simultaneously retaining part inculating crystal layer and forming core active layer non-fusible.Preferably, unfused inculating crystal layer and forming core active layer account for 5% ~ 95% of inculating crystal layer and the forming core active layer of laying in step (1).
In step (3), the thermal field controlled in crucible is cool the silicon material of molten state, carries out forming core crystallization after making it reach supercooled state.Now, grow on the seed of single crystal silicon be not completely melted by paracentral silicon liquid, grow up to the class monocrystalline with single crystal structure; The silicon liquid of close crucible wall, then based on continued growth in the small grains in crystal orientation, (110) (112), grows up to dislocation few, the efficient polycrystalline silicon that crystal boundary is appropriate.
Preferably, condensate depression is controlled in forming core crystallisation process described in step (3) for-1K ~-30K.Because the direction growth of (110) (112) is fast, thermal diffusivity is good.High supercooling degree is conducive to forming the crystal orientation be dominant with (110) (112), and simultaneously because crystal boundary is atom Cuo Pai district, dislocation glide is absorbed to grain boundaries.Appropriate crystal boundary can stop the propagation of dislocation to be expanded, and the overall dislocation of silicon ingot is reduced, thus improves the efficiency of conversion of crystalline silicon.
The present invention, by laying seed of single crystal silicon and forming core source in crucible bottom, makes to grow on the seed of single crystal silicon be not completely melted by paracentral silicon liquid, grows up to the class monocrystalline with single crystal structure; Silicon liquid near crucible wall then grows not being completely melted in forming core active layer, grows up to dislocation few, the efficient polycrystalline silicon that crystal boundary is appropriate.After tested, the battery conversion efficiency of this efficient polycrystalline silicon is higher than common polycrystalline silicon chip by 0.4% ~ 0.8%.
Second aspect, present invention also offers a kind of crystalline silicon, and described crystalline silicon obtains according to above-mentioned preparation method.
Crystalline silicon prepared by the present invention, in same silicon ingot, existing class silicon single crystal has efficient polycrystalline silicon again, and achieve the mutual supplement with each other's advantages of class monocrystalline and high-efficiency polycrystalline, cost is low, and the efficiency of conversion of the solar cell of preparation also improves greatly.
Compared to prior art, the present invention has following beneficial effect:
(1) only lay seed of single crystal silicon in crucible bottom center, decrease the consumption of seed of single crystal silicon, save production cost;
(2) by laying forming core source in crucible bottom periphery, the silicon liquid near crucible wall is made to obtain high-efficiency polycrystalline exceeding under cold state growth in forming core active layer, improve the quality near crucible wall region silico briquette, the battery conversion efficiency of overall silicon ingot is promoted greatly.
(3) crystalline silicon prepared, in same silicon ingot, existing class silicon single crystal has efficient polycrystalline silicon again, achieves the mutual supplement with each other's advantages of class monocrystalline and high-efficiency polycrystalline.
Accompanying drawing explanation
In order to be illustrated more clearly in technical scheme of the present invention, be briefly described to the accompanying drawing used required in embodiment below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
The schematic diagram that when Fig. 1 is prior art production class silicon single crystal, seed of single crystal silicon is laid in crucible bottom;
Fig. 2 is the structural representation of the class silicon single crystal that prior art is produced;
Fig. 3 is the schematic diagram that seed of single crystal silicon of the present invention and forming core source are laid in crucible bottom;
Fig. 4 is the structural representation of crystalline silicon prepared by the present invention.
Embodiment
The following stated is the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications are also considered as protection scope of the present invention.
Embodiment one
A preparation method for crystalline silicon, comprises the following steps:
(1) lay seed of single crystal silicon at random at crucible bottom center, form inculating crystal layer, the crystal orientation of described seed of single crystal silicon is not limit; Forming core source is laid at all the other positions, bottom, forms forming core active layer;
Wherein, seed of single crystal silicon is the square seed of single crystal silicon of thickness 10mm, totally 9 pieces, and the form arranged by 3 row 3 is arranged closely in the place of bottom centre of crucible.Forming core source is laid at all the other positions, bottom: evenly lay 10kg forming core source at seed of single crystal silicon square enclosure, and flattening gently and forming thickness is the forming core active layer of 10mm, the silica powder of to be particle diameter be in forming core source 10um.
Fig. 3 is the schematic diagram that seed of single crystal silicon of the present invention and forming core source are laid in crucible bottom, and wherein 1 is crucible, and 2 is seed of single crystal silicon, and 3 is forming core source.
(2) the silicon material of molten state is set above described inculating crystal layer and forming core active layer, controls the fusing point of described crucible bottom temperature lower than described seed crystal and forming core source, described inculating crystal layer and forming core active layer are not completely melted;
Wherein, the silicon material arranging molten state above inculating crystal layer and forming core active layer is: loading solid silicon material 450kg on inculating crystal layer and forming core active layer, 1560 DEG C are heated to crucible and make the melting of solid silicon material, now, the silicon material of molten state is arranged at the surface of described inculating crystal layer and forming core active layer, the silicon material of the partially molten state on forming core active layer surface has sub-fraction to drop onto in the gap in forming core source, and exceeding rapid nucleation under cold state, obtain based on the small grains in crystal orientation, (110) (112).
Wherein, control the fusing point of described crucible bottom temperature lower than described seed crystal and forming core source, make described inculating crystal layer and forming core active layer be not completely melted for: move down heat insulating cage 2cm, heat insulating cage is separated with crucible bottom, thus not to its insulation, be 1412 DEG C to control crucible bottom temperature, now unfused inculating crystal layer and forming core active layer account for 60% of inculating crystal layer and the forming core active layer of laying in step (1).
(3) temperature in described crucible is controlled along vertical with the described crucible bottom direction gradient of rising formation temperature gradually upwards, make the silicon material forming core crystallization on described seed of single crystal silicon and forming core source after melting, formation center is the peripheral crystalline silicon for high-efficiency polycrystalline of class monocrystalline;
Because heat insulating cage is not incubated crucible bottom, heat distributes from crucible bottom, the temperature in crucible is made to form the thermograde risen gradually from the bottom to top, silicon material after fusing forms silicon liquid, grow on the seed of single crystal silicon be not completely melted by paracentral silicon liquid, grow up to the class monocrystalline with single crystal structure; The silicon liquid of close crucible wall, then based on continued growth in the small grains in crystal orientation, (110) (112), grows up to dislocation few, the efficient polycrystalline silicon that crystal boundary is appropriate.Test after the section of this efficient polycrystalline silicon, its battery conversion efficiency is higher than common polycrystalline silicon chip by 0.8%.
Fig. 4 is the structural representation of crystalline silicon prepared by the present invention.Wherein, 1 is crucible, and 2 is seed of single crystal silicon, and 3 is forming core source, and 4 is class single-crystal region, and 5 is high-efficiency polycrystalline silicon area.
Utilize crystalline silicon prepared by the present embodiment, during same silicon is fixed, existing class silicon single crystal has efficient polycrystalline silicon again, achieves the mutual supplement with each other's advantages of class monocrystalline and high-efficiency polycrystalline.Simple to operate, process costs is low, and obtained conversion efficiency of solar cell also improves greatly.
Embodiment two
A preparation method for crystalline silicon, comprises the following steps:
(1) lay seed of single crystal silicon at random at crucible bottom center, form inculating crystal layer, the crystal orientation of described seed of single crystal silicon is not limit; Forming core source is laid at all the other positions, bottom, forms forming core active layer;
Wherein, seed of single crystal silicon is the square seed of single crystal silicon of thickness 5mm, totally 16 pieces, and the form arranged by 4 row 4 is arranged closely in the place of bottom centre of crucible.Forming core source is laid at all the other positions, bottom: evenly lay 5kg forming core source at seed of single crystal silicon square enclosure, and flattening gently and forming thickness is the forming core active layer of 1mm, the silica flour of to be particle diameter be in forming core source 20um.
(2) the silicon material of molten state is set above described inculating crystal layer and forming core active layer, controls the fusing point of described crucible bottom temperature lower than described seed crystal and forming core source, described inculating crystal layer and forming core active layer are not completely melted;
Wherein, the silicon material arranging molten state above inculating crystal layer and forming core active layer is: loading solid silicon material 500kg on inculating crystal layer and forming core active layer, 1560 DEG C are heated to crucible and make the melting of solid silicon material, form silicon liquid, now, the silicon material of molten state is arranged at the surface of described inculating crystal layer and forming core active layer, the silicon material of the partially molten state on forming core active layer surface has sub-fraction to drop onto in the gap in forming core source, and exceeding rapid nucleation under cold state, obtain based on the small grains in crystal orientation, (110) (112).
Wherein, control the fusing point of described crucible bottom temperature lower than described seed crystal and forming core source, make described inculating crystal layer and forming core active layer be not completely melted for: move down heat insulating cage 5cm, heat insulating cage is separated with crucible bottom, thus not to its insulation, be 1350 DEG C to control crucible bottom temperature, now unfused inculating crystal layer and forming core active layer account for 90% of inculating crystal layer and the forming core active layer of laying in step (1).
(3) temperature in described crucible is controlled along vertical with the described crucible bottom direction gradient of rising formation temperature gradually upwards, make the silicon material forming core crystallization on described seed of single crystal silicon and forming core source after melting, formation center is the peripheral crystalline silicon for high-efficiency polycrystalline of class monocrystalline;
Because heat insulating cage is not incubated crucible bottom, heat distributes from crucible bottom, the temperature in crucible is made to form the thermograde risen gradually from the bottom to top, silicon material after fusing forms silicon liquid, grow on the seed crystal be not completely melted by paracentral silicon liquid, grow up to the class monocrystalline with single crystal structure; The silicon liquid of close crucible wall, then based on continued growth in the small grains in crystal orientation, (110) (112), grows up to dislocation few, the efficient polycrystalline silicon that crystal boundary is appropriate.Test after the section of this efficient polycrystalline silicon, its battery conversion efficiency is higher than common polycrystalline silicon chip by 0.4%.
Utilize crystalline silicon prepared by the present embodiment, during same silicon is fixed, existing class silicon single crystal has efficient polycrystalline silicon again, achieves the mutual supplement with each other's advantages of class monocrystalline and high-efficiency polycrystalline.Simple to operate, process costs is low, and obtained conversion efficiency of solar cell also improves greatly.
Embodiment three
A preparation method for crystalline silicon, comprises the following steps:
(1) lay seed of single crystal silicon at random at crucible bottom center, form inculating crystal layer, the crystal orientation of described seed of single crystal silicon is not limit; Forming core source is laid at all the other positions, bottom, forms forming core active layer;
Wherein, seed of single crystal silicon is the columnar single crystal silicon seed of thickness 50mm, totally 1 piece, be laid on the center place of the bottom of crucible, upper forming core source is filled at all the other positions, bottom, flattens forming core active layer gently and makes it thickness and be about 30mm, the carborundum powder of to be particle diameter be in forming core source 1cm.
(2) the silicon material of molten state is set above described inculating crystal layer and forming core active layer, controls the fusing point of described crucible bottom temperature lower than described seed crystal and forming core source, described inculating crystal layer and forming core active layer are not completely melted;
Wherein, the silicon material arranging molten state above inculating crystal layer and forming core active layer is: in another one crucible, heat 200kg solid silicon material, the silicon material of obtained molten state, the silicon material of this molten state is poured into above described seed of single crystal silicon, because the Thickness Ratio seed crystal thickness of forming core active layer is less, the silicon material of molten state flows in described forming core active layer from seed crystal, and have sub-fraction to drop onto in the gap in forming core source, and exceeding rapid nucleation under cold state, obtain based on the small grains in crystal orientation, (110) (112).
Wherein, control the fusing point of described crucible bottom temperature lower than described seed crystal and forming core source, make described inculating crystal layer and forming core active layer be not completely melted for: move down heat insulating cage 6cm, heat insulating cage is separated with crucible bottom, thus not to its insulation, be 1300 DEG C to control crucible bottom temperature, now unfused inculating crystal layer and forming core active layer account for 95% of inculating crystal layer and the forming core active layer of laying in step (1).
(3) temperature in described crucible is controlled along vertical with the described crucible bottom direction gradient of rising formation temperature gradually upwards, make the silicon material forming core crystallization on described seed of single crystal silicon and forming core source after melting, formation center is the peripheral crystalline silicon for high-efficiency polycrystalline of class monocrystalline;
Because heat insulating cage is not incubated crucible bottom, heat distributes from crucible bottom, the temperature in crucible is made to form the thermograde risen gradually from the bottom to top, silicon material after fusing forms silicon liquid, grow on the seed crystal be not completely melted by paracentral silicon liquid, grow up to the class monocrystalline with single crystal structure; The silicon liquid of close crucible wall, then based on continued growth in the small grains in crystal orientation, (110) (112), grows up to dislocation few, the efficient polycrystalline silicon that crystal boundary is appropriate.Test after the section of this efficient polycrystalline silicon, its battery conversion efficiency is higher than common polycrystalline silicon chip by 0.6%.
Utilize crystalline silicon prepared by the present embodiment, during same silicon is fixed, existing class silicon single crystal has efficient polycrystalline silicon again, achieves the mutual supplement with each other's advantages of class monocrystalline and high-efficiency polycrystalline.Simple to operate, process costs is low, and obtained conversion efficiency of solar cell also improves greatly.
Embodiment four
A preparation method for crystalline silicon, comprises the following steps:
(1) lay seed of single crystal silicon at random at crucible bottom center, form inculating crystal layer, the crystal orientation of described seed of single crystal silicon is not limit; Forming core source is laid at all the other positions, bottom, forms forming core active layer;
Wherein, seed of single crystal silicon is the square seed of single crystal silicon of thickness 20mm, totally 4 pieces, and the form arranged by 2 row 2 is arranged closely in the place of bottom centre of crucible.Forming core source is laid at all the other positions, bottom: evenly lay 1kg forming core source at seed of single crystal silicon square enclosure, flatten gently and form the forming core active layer that thickness is 20mm, forming core source is the mixture that carbon dust and silica powder form by 1:1, and the particle diameter of carbon dust is 0.1um, and the particle diameter of silica powder is 200um.
(2) the silicon material of molten state is set above described inculating crystal layer and forming core active layer, controls the fusing point of described crucible bottom temperature lower than described seed crystal and forming core source, described inculating crystal layer and forming core active layer are not completely melted;
Wherein, the silicon material arranging molten state above described inculating crystal layer and forming core active layer is, 200kg solid silicon material is heated in another one crucible, the silicon material of obtained molten state, the silicon material of this molten state is poured in the crucible being covered with seed of single crystal silicon and forming core source, now, the silicon material of molten state is arranged at the surface of described inculating crystal layer and forming core active layer, the silicon material of the partially molten state on forming core active layer surface has sub-fraction to drop onto in the gap in forming core source, and exceeding rapid nucleation under cold state, obtain based on the small grains in crystal orientation, (110) (112).
Wherein, control the fusing point of described crucible bottom temperature lower than described seed crystal and forming core source, concrete operations are: by be equipped with silicon liquid crucible be inserted into sidewall heating graphite furnace on, make the sidewall of crucible be close to the hot-plate of graphite furnace, and crucible bottom is just exposed outside hot-plate.Because crucible bottom is constantly dispelled the heat, temperature is controlled in 1300 DEG C, and now unfused inculating crystal layer and forming core active layer account for 95% of inculating crystal layer and the forming core active layer of laying in step (1).
(3) temperature in described crucible is controlled along vertical with the described crucible bottom direction gradient of rising formation temperature gradually upwards, make the silicon material forming core crystallization on described seed of single crystal silicon and forming core source after melting, formation center is the peripheral crystalline silicon for high-efficiency polycrystalline of class monocrystalline;
Start heating schedule to heat crucible, make it Slow cooling, and the temperature controlled in described crucible is along vertical and the described crucible bottom direction gradient of rising formation temperature gradually upwards, silicon material after fusing forms silicon liquid, grow on the seed crystal be not completely melted by paracentral silicon liquid, grow up to the class monocrystalline with single crystal structure; The silicon liquid of close crucible wall, then based on continued growth in the small grains in crystal orientation, (110) (112), grows up to dislocation few, the efficient polycrystalline silicon that crystal boundary is appropriate.
Utilize crystalline silicon prepared by the present embodiment, during same silicon is fixed, existing class silicon single crystal has efficient polycrystalline silicon again, achieves the mutual supplement with each other's advantages of class monocrystalline and high-efficiency polycrystalline.Simple to operate, process costs is low, and obtained conversion efficiency of solar cell also improves greatly.
Claims (9)
1. a preparation method for crystalline silicon, is characterized in that, comprises the following steps:
(1) lay seed of single crystal silicon at random at crucible bottom center, form inculating crystal layer, the crystal orientation of described seed of single crystal silicon is not limit; Forming core source is laid at all the other positions, bottom, forms forming core active layer;
(2) the silicon material of molten state is set on described inculating crystal layer and forming core active layer, controls the fusing point of described crucible bottom temperature lower than described seed crystal and forming core source, described inculating crystal layer and forming core active layer are not completely melted;
(3) temperature in described crucible is controlled along vertical with the described crucible bottom direction gradient of rising formation temperature gradually upwards, make the silicon material forming core crystallization on described seed of single crystal silicon and forming core source after melting, formation center is the peripheral crystalline silicon for high-efficiency polycrystalline of class monocrystalline; Condensate depression is controlled for-1K ~-30K in forming core crystallisation process described in step (3).
2. the preparation method of a kind of crystalline silicon according to claim 1, is characterized in that, the seed of single crystal silicon described in step (1) is square or circular arrangement at crucible bottom center, close contact between seed of single crystal silicon and seed crystal.
3. the preparation method of a kind of crystalline silicon according to claim 1, is characterized in that, the thickness of the inculating crystal layer described in step (1) is 5 ~ 50mm.
4. the preparation method of a kind of crystalline silicon according to claim 1, is characterized in that, described in step (1), the particle diameter in forming core source is 0.1um ~ 1cm.
5. the preparation method of a kind of crystalline silicon according to claim 1, is characterized in that, described in step (1), the thickness of forming core active layer is 1 ~ 30mm.
6. the preparation method of a kind of crystalline silicon according to claim 1, it is characterized in that, forming core source described in step (1) is selected from silica flour, the silicon based compound close with the lattice of silicon material and react one or more in the material generating silicon based compound with silicon material, or silica flour, and the close silicon based compound of the lattice of silicon material and react the mixture of one or more and silicon nitride in the material generating silicon based compound with silicon material.
7. the preparation method of a kind of crystalline silicon according to claim 1, it is characterized in that, the silicon material arranging molten state in step (2) above described inculating crystal layer and forming core active layer is: loading solid silicon material above described inculating crystal layer and forming core active layer, heating is carried out to described crucible and makes the melting of described silicon material, now, the silicon material of described molten state is arranged at the surface of described inculating crystal layer and forming core active layer.
8. the preparation method of a kind of crystalline silicon according to claim 1, it is characterized in that, the silicon material arranging molten state in step (2) above described inculating crystal layer and forming core active layer is: heat solid silicon material in another one crucible, the silicon material of obtained molten state, be equipped with in the crucible of inculating crystal layer and forming core active layer described in the silicon material of described molten state is poured into, now, the silicon material of described molten state is arranged at the surface of described inculating crystal layer and forming core active layer.
9. a crystalline silicon, is characterized in that, described crystalline silicon is obtained by any one method in claim 1-8.
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| CN103526278B (en) * | 2013-10-10 | 2015-11-04 | 西华大学 | A kind of method and apparatus of casting single crystal silicon ingot |
| CN103834994A (en) * | 2014-03-13 | 2014-06-04 | 江西赛维Ldk太阳能高科技有限公司 | Polycrystalline silicon ingot and preparation method thereof and polycrystalline silicon wafer |
| CN104532343B (en) * | 2014-11-07 | 2017-06-06 | 江苏美科硅能源有限公司 | The preparation method and its fritting high-efficiency seed crystal of a kind of efficient ingot of fritting retain accessory plate |
| CN105568374A (en) * | 2016-03-16 | 2016-05-11 | 常熟华融太阳能新型材料有限公司 | Selective all-melting high-efficiency crucible for polycrystal cast ingots |
| CN105755537B (en) * | 2016-04-14 | 2018-04-17 | 江西赛维Ldk太阳能高科技有限公司 | A kind of polycrystal silicon ingot and preparation method thereof |
| GB2550415A (en) * | 2016-05-18 | 2017-11-22 | Rec Solar Pte Ltd | Silicon ingot growth crucible with patterned protrusion structured layer |
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| CN109972197A (en) * | 2019-03-06 | 2019-07-05 | 赛维Ldk太阳能高科技(新余)有限公司 | A kind of monocrystalline silicon cast ingot crucible and monocrystalline silicon cast ingot method |
| CN110295391A (en) * | 2019-07-31 | 2019-10-01 | 江苏协鑫硅材料科技发展有限公司 | The preparation method of crystalline silicon ingot |
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| JPH11236291A (en) * | 1998-02-25 | 1999-08-31 | Mitsubishi Materials Corp | Crucible for producing silicon ingot having unidirectionally solidified polycrystalline structure |
| CN102277618A (en) * | 2011-07-28 | 2011-12-14 | 英利能源（中国）有限公司 | Polysilicon ingot, manufacturing method and growing furnace thereof, as well as bottom plate and solar cell of growing furnace |
| CN102534772A (en) * | 2012-02-28 | 2012-07-04 | 江苏协鑫硅材料科技发展有限公司 | Method for growing large-grain cast polycrystalline silicon |
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