CN102877129A - Crystalline silicon and preparation method thereof - Google Patents
Crystalline silicon and preparation method thereof Download PDFInfo
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- CN102877129A CN102877129A CN2012103333089A CN201210333308A CN102877129A CN 102877129 A CN102877129 A CN 102877129A CN 2012103333089 A CN2012103333089 A CN 2012103333089A CN 201210333308 A CN201210333308 A CN 201210333308A CN 102877129 A CN102877129 A CN 102877129A
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Abstract
The invention discloses a preparation method of crystalline silicon, which comprises the following steps: a mono-crystal silicon seed crystal is randomly paved in the center of the bottom of a crucible to form a seed crystal layer; a nucleation source is paved at the residual part of the bottom to form a nucleation source layer; a silicon material in a melting state is arranged on the seed crystal layer and the nucleation source layer to control the temperature of the bottom of the crucible so as to prevent the seed crystal layer and the nucleation source layer from being completely molten; and the temperature in the crucible is controlled to gradually increase to form temperature gradient in the direction vertical to the upward direction of the bottom of the crucible, so that the molten silicone material can form nuclear crystallization on the mono-crystal silicone seed crystal and the nucleation source and the crystalline silicon of which the center is mono-like and the periphery is high-effective polycrystal. The invention further discloses the crystalline silicon prepared by the preparation method for crystalline silicon. The preparation method for crystalline silicon reduces the consumption of the mono-crystal silicone seed crystal, saves the production cost, improves the quality of the silicon block in the area close to the side wall of the crucible; and monocrystal-like silicon and high-effective polycrystal silicone coexist in the prepared crystalline silicone, and the complementary advantages of the monocrystal-like silicone and the high-effective polycrystal silicone are realized.
Description
Technical field
The present invention relates to the semi-conductor preparation field, especially a kind of crystalline silicon that contains simultaneously class monocrystalline and efficient polycrystalline and preparation method thereof.
Background technology
Crystalline silicon is to use the most general semiconductor material during solar cell is made, and the crystalline silicon for the manufacture of solar cell mainly is the polysilicon that adopts the silicon single crystal of vertical pulling method and adopt ingot casting technology at present.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; The pulling of silicon single crystal efficiency of conversion is high, but that single feeds intake is few, complicated operation, and cost is high.How both are united two into one, form mutual supplement with each other's advantages, become focus and the difficult point of present photovoltaic industry development.Under this background, the class monocrystalline between polysilicon and silicon single crystal has progressed into people's the visual field.
Class monocrystalline (Mono Like) is called again accurate monocrystalline, is based on the technique of polycrystalline cast ingot, uses single crystal seed by part in long brilliant process, obtains the polysilicon chip that outward appearance and electrical property all are similar to monocrystalline.The class monocrystalline silicon piece to the efficiency of conversion of sun power far above polysilicon, even silicon single crystal shoulder to shoulder, but its manufacturing process and polysilicon are similar, manufacturing cost is low and silicon single crystal significantly, thereby become rapidly the manufacturing new lover of solar cell.
Yet, the at present production of class monocrystalline silicon piece there is no ripe technique, generally be to be paved with seed of single crystal silicon (such as Fig. 1) in crucible bottom first in the prior art, and then fill the silicon material, passing through heating and melting and controlling the crucible bottom temperature is not melted seed crystal fully, so that silicon liquid is grown at the seed crystal that is not melted fully, grow the class monocrystalline with single crystal structure.This technique not only consumption of seed crystal is large, and manufacturing cost is high, and because homogeneity and the directional property of thermal field, is difficult to grow monocrystalline near the zone of crucible wall, and most of zone is polycrystalline (such as Fig. 2), has had a strong impact on the ratio of monocrystalline.Because this zone is the zone of monocrystalline and polycrystalline coexistence, crystal grain pushes mutually, and dislocation is very easily expanded and bred, and causes this regional silico briquette of poor quality, and battery conversion efficiency is low, even is lower than common polysilicon 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 method not only consumption of seed crystal further reduces, and has greatly improved the quality of the regional silico briquette of close crucible wall.The present invention also discloses the crystalline silicon that obtains by this preparation method simultaneously.
First aspect the invention provides a kind of preparation method of crystalline silicon, may further comprise the steps:
(1) lay at random seed of single crystal silicon at the crucible bottom center, form inculating crystal layer, the crystal orientation of described seed of single crystal silicon is not limit; The forming core source is laid at all the other positions, bottom, forms forming core source layer;
(2) the silicon material of molten state is set at described inculating crystal layer and forming core source layer, control described crucible bottom temperature be lower than described seed crystal and forming core source fusing point so that described inculating crystal layer and forming core source layer are not completely melted;
(3) temperature of control in the described crucible is along the vertical direction that makes progress with the described crucible bottom formation temperature gradient that rises gradually, so that the silicon material forming core crystallization on described seed of single crystal silicon and forming core source after the fusing, the formation center is that class monocrystalline periphery is the crystalline silicon of efficient polycrystalline;
Preferably, the described seed of single crystal silicon of step (1) is square or circular arrangement at the crucible bottom center, close contact between seed of single crystal silicon and the seed crystal.
Preferably, the thickness of the described inculating crystal layer of step (1) is 5 ~ 50mm.
Preferably, the particle diameter in forming core source is 0.1um ~ 1cm described in the step (1).
Preferably, the thickness of forming core source layer is 1～30mm described in the step (1).
Preferably, the silicon based compound that forming core source described in the step (1) is selected from silica flour, approach with the lattice of silicon material and generate in the material of silicon based compound one or more with the reaction of silicon material, or silica flour, the silicon based compound that approaches with the lattice of silicon material and generate one or more and the mixture of silicon nitride in the material of silicon based compound with the reaction of silicon material.
More preferably, the approaching silicon based compound of lattice described and the silicon material is carborundum powder or silica powder.
More preferably, described material with silicon material reaction generation silicon based compound is carbon dust.
Preferably, the silicon material that at described inculating crystal layer and forming core source layer molten state is set in the step (2) is: loading solid silicon material above described inculating crystal layer and forming core source layer, described crucible is heated so that described silicon material melting forms silicon liquid, at this moment, the silicon material of described molten state is arranged at the surface of described inculating crystal layer and forming core source layer.Also preferably, the silicon material that at described inculating crystal layer and forming core source layer molten state is set in the step (2) is: heat solid silicon material in the another one crucible, make the silicon material of molten state, the silicon material of described molten state is poured in the described crucible that is equipped with forming core source layer, at this moment, the silicon material of described molten state is arranged at the surface of described inculating crystal layer and forming core source layer.
In the step (2), the silicon material that is arranged on the molten state on layer surface, forming core source has sub-fraction to drop onto in the slit in forming core source, and exceeds rapid nucleation under the cold state, and obtaining take crystal orientation, (110) (112) is main small grains.
The described inculating crystal layer of step (2) and forming core source layer are not completely melted and refer to part inculating crystal layer and the fusing of forming core source layer, and retaining part inculating crystal layer and forming core source layer do not melt simultaneously.Preferably, unfused inculating crystal layer and forming core source layer account for 5% ~ 95% of the middle inculating crystal layer of laying of step (1) and forming core source layer.
In the step (3), the thermal field of control in the crucible be for the silicon material to molten state cools off, and carries out the forming core crystallization after making it reach supercooled state.At this moment, grow at the seed of single crystal silicon that is not completely melted by paracentral silicon liquid, grow up to the class monocrystalline with single crystal structure; Near the then continued growth on take crystal orientation, (110) (112) as main small grains of the silicon liquid of crucible wall, grow up to dislocation few, the efficient polysilicon that crystal boundary is an amount of.
Preferably, described in the step (3) in the forming core crystallisation process control condensate depression be-1K ~-30K.Because the growth of the direction of (110) (112) is fast, thermal diffusivity is good.High supercooling degree is conducive to form the crystal orientation that is dominant with (110) (112), because crystal boundary is atom mistake row district, dislocation glide is absorbed to grain boundaries simultaneously.An amount of crystal boundary can stop the propagation expansion of dislocation, so that the whole dislocation minimizing of silicon ingot, thereby the efficiency of conversion of raising crystalline silicon.
The present invention so that grow at the seed of single crystal silicon that is not completely melted by paracentral silicon liquid, grows up to the class monocrystalline with single crystal structure by laying seed of single crystal silicon and forming core source in crucible bottom; Silicon liquid near crucible wall is then grown at the forming core source layer that is not completely melted, and grows up to dislocation few, the efficient polysilicon that crystal boundary is an amount of.After tested, the battery conversion efficiency of this efficient polysilicon is higher by 0.4% ~ 0.8% than common polysilicon chip.
Second aspect, the present invention also provides a kind of crystalline silicon, and described crystalline silicon makes according to above-mentioned preparation method.
The crystalline silicon of the present invention's preparation, existing class silicon single crystal has again efficient polysilicon in the same silicon ingot, has realized the mutual supplement with each other's advantages of class monocrystalline and efficient polycrystalline, and cost is low, and the efficiency of conversion of the solar cell of preparation also improves greatly.
Than prior art, the present invention has following beneficial effect:
(1) only lays seed of single crystal silicon in the crucible bottom center, reduced the consumption of seed of single crystal silicon, saved production cost;
(2) by laying the forming core source in the crucible bottom periphery, so that obtain efficient polycrystalline in the growth of forming core source layer near the silicon liquid of crucible wall exceeding under the cold state, improved the quality of close crucible wall zone silico briquette, so that the battery conversion efficiency of whole silicon ingot promotes greatly.
(3) crystalline silicon of preparation, existing class silicon single crystal has again efficient polysilicon in the same silicon ingot, has realized the mutual supplement with each other's advantages of class monocrystalline and efficient polycrystalline.
Description of drawings
In order to be illustrated more clearly in technical scheme of the present invention, the below will do to introduce simply to the accompanying drawing of required use in the embodiment, apparently, accompanying drawing in the following describes only is some embodiments of the present invention, for those of ordinary skills, under the prerequisite of not paying creative work, can also obtain according to these accompanying drawings other accompanying drawing.
The schematic diagram that seed of single crystal silicon was laid in crucible bottom when Fig. 1 was prior art production class silicon single crystal;
Fig. 2 is the structural representation of the class silicon single crystal of prior art production;
Fig. 3 is the schematic diagram that lay in crucible bottom in seed of single crystal silicon of the present invention and forming core source;
Fig. 4 is the structural representation of the crystalline silicon for preparing of the present invention.
Embodiment
The following stated is preferred implementation of the present invention; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention; can also make some improvements and modifications, these improvements and modifications also are considered as protection scope of the present invention.
Embodiment one
A kind of preparation method of crystalline silicon may further comprise the steps:
(1) lay at random seed of single crystal silicon at the crucible bottom center, form inculating crystal layer, the crystal orientation of described seed of single crystal silicon is not limit; The forming core source is laid at all the other positions, bottom, forms forming core source layer;
Wherein, seed of single crystal silicon is the square seed of single crystal silicon of thickness 10mm, totally 9, locates in the bottom centre of crucible by the form close-packed arrays of 3 row, 3 row.The forming core source is laid at all the other positions, bottom: in the peripheral 10kg forming core source of evenly laying of seed of single crystal silicon square, flattening gently and forming thickness is the forming core source layer of 10mm, and the forming core source is that particle diameter is the silica powder of 10um.
Fig. 3 is the schematic diagram that lay in crucible bottom in seed of single crystal silicon of the present invention and forming core source, and wherein 1 is crucible, and 2 is seed of single crystal silicon, and 3 is the forming core source.
(2) the silicon material of molten state is set above described inculating crystal layer and forming core source layer, controls the fusing point that described crucible bottom temperature is lower than described seed crystal and forming core source, so that described inculating crystal layer and forming core source layer are not completely melted;
Wherein, at the silicon material that molten state is set above inculating crystal layer and the forming core source layer be: loading solid silicon material 450kg on inculating crystal layer and forming core source layer, crucible is heated to 1560 ℃ so that the melting of solid silicon material, at this moment, the silicon material of molten state is arranged at the surface of described inculating crystal layer and forming core source layer, the silicon material of the lip-deep partially molten state of forming core source layer has sub-fraction to drop onto in the slit in forming core source, and exceeding rapid nucleation under the cold state, obtaining take crystal orientation, (110) (112) is main small grains.
Wherein, control the fusing point that described crucible bottom temperature is lower than described seed crystal and forming core source, so that described inculating crystal layer and forming core source layer be not completely melted for: move down heat insulating cage 2cm, so that the heat insulating cage separates with crucible bottom, thereby not to its insulation, take control crucible bottom temperature as 1412 ℃, this moment, unfused inculating crystal layer and forming core source layer accounted for 60% of the middle inculating crystal layer of laying of step (1) and forming core source layer.
(3) temperature of control in the described crucible is along the vertical direction that makes progress with the described crucible bottom formation temperature gradient that rises gradually, so that the silicon material forming core crystallization on described seed of single crystal silicon and forming core source after the fusing, the formation center is that class monocrystalline periphery is the crystalline silicon of efficient polycrystalline;
Because the heat insulating cage is not incubated crucible bottom, heat distributes from crucible bottom, so that the temperature in the crucible forms the thermograde that rises gradually from the bottom to top, silicon material after the fusing forms silicon liquid, grow at the seed of single crystal silicon that is not completely melted by paracentral silicon liquid, grow up to the class monocrystalline with single crystal structure; Near the then continued growth on take crystal orientation, (110) (112) as main small grains of the silicon liquid of crucible wall, grow up to dislocation few, the efficient polysilicon that crystal boundary is an amount of.Test after this efficient polysilicon section, its battery conversion efficiency is higher by 0.8% than common polysilicon chip.
Fig. 4 is the structural representation of the crystalline silicon for preparing of the present invention.Wherein, 1 is crucible, and 2 is seed of single crystal silicon, and 3 is the forming core source, and 4 is the class single-crystal region, and 5 is efficient multi-crystal silicon area.
Utilize the crystalline silicon of the present embodiment preparation, existing class silicon single crystal had again efficient polysilicon during same silicon was fixed, had realized the mutual supplement with each other's advantages of class monocrystalline and efficient polycrystalline.Simple to operate, process costs is low, and the conversion efficiency of solar cell that makes also improves greatly.
Embodiment two
A kind of preparation method of crystalline silicon may further comprise the steps:
(1) lay at random seed of single crystal silicon at the crucible bottom center, form inculating crystal layer, the crystal orientation of described seed of single crystal silicon is not limit; The forming core source is laid at all the other positions, bottom, forms forming core source layer;
Wherein, seed of single crystal silicon is the square seed of single crystal silicon of thickness 5mm, totally 16, locates in the bottom centre of crucible by the form close-packed arrays of 4 row, 4 row.The forming core source is laid at all the other positions, bottom: in the peripheral 5kg forming core source of evenly laying of seed of single crystal silicon square, flattening gently and forming thickness is the forming core source layer of 1mm, and the forming core source is that particle diameter is the silica flour of 20um.
(2) the silicon material of molten state is set above described inculating crystal layer and forming core source layer, controls the fusing point that described crucible bottom temperature is lower than described seed crystal and forming core source, so that described inculating crystal layer and forming core source layer are not completely melted;
Wherein, at the silicon material that molten state is set above inculating crystal layer and the forming core source layer be: loading solid silicon material 500kg on inculating crystal layer and forming core source layer, crucible is heated to 1560 ℃ so that the melting of solid silicon material, form silicon liquid, at this moment, the silicon material of molten state is arranged at the surface of described inculating crystal layer and forming core source layer, the silicon material of the lip-deep partially molten state of forming core source layer has sub-fraction to drop onto in the slit in forming core source, and exceeding rapid nucleation under the cold state, obtaining take crystal orientation, (110) (112) is main small grains.
Wherein, control the fusing point that described crucible bottom temperature is lower than described seed crystal and forming core source, so that described inculating crystal layer and forming core source layer be not completely melted for: move down heat insulating cage 5cm, so that the heat insulating cage separates with crucible bottom, thereby not to its insulation, take control crucible bottom temperature as 1350 ℃, this moment, unfused inculating crystal layer and forming core source layer accounted for 90% of the middle inculating crystal layer of laying of step (1) and forming core source layer.
(3) temperature of control in the described crucible is along the vertical direction that makes progress with the described crucible bottom formation temperature gradient that rises gradually, so that the silicon material forming core crystallization on described seed of single crystal silicon and forming core source after the fusing, the formation center is that class monocrystalline periphery is the crystalline silicon of efficient polycrystalline;
Because the heat insulating cage is not incubated crucible bottom, heat distributes from crucible bottom, so that the temperature in the crucible forms the thermograde that rises gradually from the bottom to top, silicon material after the fusing forms silicon liquid, grow at the seed crystal that is not completely melted by paracentral silicon liquid, grow up to the class monocrystalline with single crystal structure; Near the then continued growth on take crystal orientation, (110) (112) as main small grains of the silicon liquid of crucible wall, grow up to dislocation few, the efficient polysilicon that crystal boundary is an amount of.Test after this efficient polysilicon section, its battery conversion efficiency is higher by 0.4% than common polysilicon chip.
Utilize the crystalline silicon of the present embodiment preparation, existing class silicon single crystal had again efficient polysilicon during same silicon was fixed, had realized the mutual supplement with each other's advantages of class monocrystalline and efficient polycrystalline.Simple to operate, process costs is low, and the conversion efficiency of solar cell that makes also improves greatly.
Embodiment three
A kind of preparation method of crystalline silicon may further comprise the steps:
(1) lay at random seed of single crystal silicon at the crucible bottom center, form inculating crystal layer, the crystal orientation of described seed of single crystal silicon is not limit; The forming core source is laid at all the other positions, bottom, forms forming core source layer;
Wherein, seed of single crystal silicon is the columnar single crystal silicon seed of thickness 50mm, totally 1, be laid on the place, center of the bottom of crucible, upper forming core sources are filled at all the other positions, bottom, flatten gently forming core source layer and make it thickness and be about 30mm, and the forming core source is that particle diameter is the carborundum powder of 1cm.
(2) the silicon material of molten state is set above described inculating crystal layer and forming core source layer, controls the fusing point that described crucible bottom temperature is lower than described seed crystal and forming core source, so that described inculating crystal layer and forming core source layer are not completely melted;
Wherein, the silicon material that molten state is set above inculating crystal layer and forming core source layer is: heating 200kg solid silicon material in the another one crucible, make the silicon material of molten state, the silicon material of this molten state is poured into described seed of single crystal silicon top, because the Thickness Ratio seed crystal thickness of forming core source layer is less, the silicon material of molten state flows on the layer of described forming core source from seed crystal, and there is sub-fraction to drop onto in the slit in forming core source, and exceeding rapid nucleation under the cold state, obtaining take crystal orientation, (110) (112) is main small grains.
Wherein, control the fusing point that described crucible bottom temperature is lower than described seed crystal and forming core source, so that described inculating crystal layer and forming core source layer be not completely melted for: move down heat insulating cage 6cm, so that the heat insulating cage separates with crucible bottom, thereby not to its insulation, take control crucible bottom temperature as 1300 ℃, this moment, unfused inculating crystal layer and forming core source layer accounted for 95% of the middle inculating crystal layer of laying of step (1) and forming core source layer.
(3) temperature of control in the described crucible is along the vertical direction that makes progress with the described crucible bottom formation temperature gradient that rises gradually, so that the silicon material forming core crystallization on described seed of single crystal silicon and forming core source after the fusing, the formation center is that class monocrystalline periphery is the crystalline silicon of efficient polycrystalline;
Because the heat insulating cage is not incubated crucible bottom, heat distributes from crucible bottom, so that the temperature in the crucible forms the thermograde that rises gradually from the bottom to top, silicon material after the fusing forms silicon liquid, grow at the seed crystal that is not completely melted by paracentral silicon liquid, grow up to the class monocrystalline with single crystal structure; Near the then continued growth on take crystal orientation, (110) (112) as main small grains of the silicon liquid of crucible wall, grow up to dislocation few, the efficient polysilicon that crystal boundary is an amount of.Test after this efficient polysilicon section, its battery conversion efficiency is higher by 0.6% than common polysilicon chip.
Utilize the crystalline silicon of the present embodiment preparation, existing class silicon single crystal had again efficient polysilicon during same silicon was fixed, had realized the mutual supplement with each other's advantages of class monocrystalline and efficient polycrystalline.Simple to operate, process costs is low, and the conversion efficiency of solar cell that makes also improves greatly.
Embodiment four
A kind of preparation method of crystalline silicon may further comprise the steps:
(1) lay at random seed of single crystal silicon at the crucible bottom center, form inculating crystal layer, the crystal orientation of described seed of single crystal silicon is not limit; The forming core source is laid at all the other positions, bottom, forms forming core source layer;
Wherein, seed of single crystal silicon is the square seed of single crystal silicon of thickness 20mm, totally 4, locates in the bottom centre of crucible by the form close-packed arrays of 2 row, 2 row.The forming core source is laid at all the other positions, bottom: in the peripheral 1kg forming core source of evenly laying of seed of single crystal silicon square, flattening gently and forming thickness is the forming core source layer of 20mm, the 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 source layer, controls the fusing point that described crucible bottom temperature is lower than described seed crystal and forming core source, so that described inculating crystal layer and forming core source layer are not completely melted;
Wherein, the silicon material that molten state is set above described inculating crystal layer and forming core source layer is, heating 200kg solid silicon material in the another one crucible, make the silicon material of molten state, the silicon material of this molten state is poured in the crucible that is covered with seed of single crystal silicon and forming core source, at this moment, the silicon material of molten state is arranged at the surface of described inculating crystal layer and forming core source layer, the silicon material of the lip-deep partially molten state of forming core source layer has sub-fraction to drop onto in the slit in forming core source, and exceeding rapid nucleation under the cold state, obtaining take crystal orientation, (110) (112) is main small grains.
Wherein, control the fusing point that described crucible bottom temperature is lower than described seed crystal and forming core source, concrete operations are: will be equipped with silicon liquid crucible be inserted on the graphite furnace of sidewall heating, 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 ℃, and this moment, unfused inculating crystal layer and forming core source layer accounted for 95% of the middle inculating crystal layer of laying of step (1) and forming core source layer.
(3) temperature of control in the described crucible is along the vertical direction that makes progress with the described crucible bottom formation temperature gradient that rises gradually, so that the silicon material forming core crystallization on described seed of single crystal silicon and forming core source after the fusing, the formation center is that class monocrystalline periphery is the crystalline silicon of efficient polycrystalline;
Starting heating schedule heats crucible, make it Slow cooling, and control temperature in the described crucible along the vertical direction that makes progress with the described crucible bottom formation temperature gradient that rises gradually, silicon material after the fusing forms silicon liquid, grow at the seed crystal that is not completely melted by paracentral silicon liquid, grow up to the class monocrystalline with single crystal structure; Near the then continued growth on take crystal orientation, (110) (112) as main small grains of the silicon liquid of crucible wall, grow up to dislocation few, the efficient polysilicon that crystal boundary is an amount of.
Utilize the crystalline silicon of the present embodiment preparation, existing class silicon single crystal had again efficient polysilicon during same silicon was fixed, had realized the mutual supplement with each other's advantages of class monocrystalline and efficient polycrystalline.Simple to operate, process costs is low, and the conversion efficiency of solar cell that makes also improves greatly.
Claims (10)
1. the preparation method of a crystalline silicon is characterized in that, may further comprise the steps:
(1) lay at random seed of single crystal silicon at the crucible bottom center, form inculating crystal layer, the crystal orientation of described seed of single crystal silicon is not limit; The forming core source is laid at all the other positions, bottom, forms forming core source layer;
(2) the silicon material of molten state is set at described inculating crystal layer and forming core source layer, controls the fusing point that described crucible bottom temperature is lower than described seed crystal and forming core source, so that described inculating crystal layer and forming core source layer are not completely melted;
(3) temperature of control in the described crucible is along the vertical direction that makes progress with the described crucible bottom formation temperature gradient that rises gradually, so that the silicon material forming core crystallization on described seed of single crystal silicon and forming core source after the fusing, the formation center is that class monocrystalline periphery is the crystalline silicon of efficient polycrystalline.
2. the preparation method of a kind of crystalline silicon according to claim 1 is characterized in that, the described seed of single crystal silicon of step (1) is square or circular arrangement at the crucible bottom center, close contact between seed of single crystal silicon and the seed crystal.
3. the preparation method of a kind of crystalline silicon according to claim 1 is characterized in that, the thickness of the described inculating crystal layer of step (1) is 5 ~ 50mm.
4. the preparation method of a kind of crystalline silicon according to claim 1 is characterized in that, the particle diameter in forming core source is 0.1um ~ 1cm described in the step (1).
5. the preparation method of a kind of crystalline silicon according to claim 1 is characterized in that, the thickness of forming core source layer is 1～30mm described in the step (1).
6. the preparation method of a kind of crystalline silicon according to claim 1, it is characterized in that, the silicon based compound that forming core source described in the step (1) is selected from silica flour, approach with the lattice of silicon material and generate in the material of silicon based compound one or more with the reaction of silicon material, or silica flour, the silicon based compound that approaches with the lattice of silicon material and generate one or more and the mixture of silicon nitride in the material of silicon based compound with the reaction of silicon material.
7. the preparation method of a kind of crystalline silicon according to claim 1, it is characterized in that, in the step (2) at the silicon material that molten state is set above described inculating crystal layer and the forming core source layer be: loading solid silicon material above described inculating crystal layer and forming core source layer, described crucible is heated so that the melting of described silicon material, at this moment, the silicon material of described molten state is arranged at the surface of described inculating crystal layer and forming core source layer.
8. the preparation method of a kind of crystalline silicon according to claim 1, it is characterized in that, the silicon material that molten state is set above described inculating crystal layer and forming core source layer in the step (2) is: heat solid silicon material in the another one crucible, make the silicon material of molten state, the silicon material of described molten state is poured in the described crucible that is equipped with inculating crystal layer and forming core source layer, at this moment, the silicon material of described molten state is arranged at the surface of described inculating crystal layer and forming core source layer.
9. the preparation method of a kind of crystalline silicon according to claim 1 is characterized in that, control condensate depression described in the step (3) in the forming core crystallisation process to be-1K ~-30K.
10. a crystalline silicon is characterized in that, described crystalline silicon makes by any one method among the claim 1-9.
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| CN108396376A (en) * | 2017-07-18 | 2018-08-14 | 陕西西京电子科技有限公司 | The preparation method of one type monocrystalline and the mixing silicon ingot of high-efficiency polycrystalline |
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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 |
| CN104532343A (en) * | 2014-11-07 | 2015-04-22 | 江苏美科硅能源有限公司 | Aemi-molten high-efficiency ingot preparation method and semi-molten high-efficiency seed crystal retention auxiliary board |
| 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 |
| CN105755537A (en) * | 2016-04-14 | 2016-07-13 | 江西赛维Ldk太阳能高科技有限公司 | Polycrystalline silicon ingot and production method thereof |
| 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 |
| US20200010978A1 (en) * | 2016-05-18 | 2020-01-09 | Rec Solar Pte. Ltd. | Silicon ingot growth crucible with patterned protrusion structured layer |
| CN108396376A (en) * | 2017-07-18 | 2018-08-14 | 陕西西京电子科技有限公司 | The preparation method of one type monocrystalline and the mixing silicon ingot of high-efficiency polycrystalline |
| 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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