CN108866623A - A kind of polycrystalline silicon ingot casting method - Google Patents
A kind of polycrystalline silicon ingot casting method Download PDFInfo
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- CN108866623A CN108866623A CN201810751738.XA CN201810751738A CN108866623A CN 108866623 A CN108866623 A CN 108866623A CN 201810751738 A CN201810751738 A CN 201810751738A CN 108866623 A CN108866623 A CN 108866623A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/04—Production of homogeneous polycrystalline material with defined structure from liquids
- C30B28/08—Production of homogeneous polycrystalline material with defined structure from liquids by zone-melting
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Abstract
The invention discloses a kind of polycrystalline silicon ingot casting methods, including：Multiple monocrystalline silicon pieces being arranged in array are laid in crucible bottom, there is default spacing between adjacent single crystalline silicon wafer；Polycrysalline silcon is filled in default spacing；Silicon material is placed on monocrystalline silicon piece, crucible is heated, and makes melting silicon materials；After all melting silicon materials, stop heating, the silicon material for controlling molten condition forms polycrystal silicon ingot in monocrystalline silicon sheet surface nucleating growth.Polycrystalline silicon ingot casting method provided by the present invention, using monocrystalline silicon piece as seed crystal, since monocrystalline dislocation is low, monocrystalline silicon sheet surface epitaxial growth crystal inherits monocrystalline low dislocation feature, crystal bottom dislocation etching pits are fundamentally reduced, to reach fast lifting silicon wafer transformation efficiency result.
Description
Technical field
The present invention relates to field of polycrystalline silicon ingot, more particularly to a kind of polycrystalline silicon ingot casting method.
Background technique
Solar energy resources are abundant, widely distributed, are most potential renewable energy.Solar energy power generating is because of it
The features such as cleaning, be safe and convenient, efficient, it has also become countries in the world common concern and the new industry given priority to.
It is one of polycrystalline silicon casting ingot process that polycrystalline, which partly melts technique, mainly uses fine particle silicon or fragment place mat crucible
Bottom, heating, fusing, and grow silicon liquid parent phase in seed crystal face fast nucleation；Currently, being spread in half process of smelting in crucible bottom
If seed crystal generally uses monocrystalline or polycrystalline particle to be laid with as seed crystal, but there is a problem of that finished product conversion ratio is low and dislocation defects
High problem.
Summary of the invention
The object of the present invention is to provide a kind of polycrystalline silicon ingot casting methods, solve finished product present in current polycrystalline silicon ingot casting
Rate is low, and there is a problem of that dislocation defects are high.
In order to solve the above technical problems, the present invention provides a kind of polycrystalline silicon ingot casting method, including：
Multiple monocrystalline silicon pieces being arranged in array are laid in crucible bottom, are had between presetting between the adjacent monocrystalline silicon piece
Away from；
Polycrysalline silcon is filled in the default spacing；
Silicon material is placed on the monocrystalline silicon piece, the crucible is heated, makes the melting silicon materials；
After all melting silicon materials, stops heating, control the silicon material of molten condition in the monocrystalline silicon piece table
Face nucleating growth forms polycrystal silicon ingot.
Wherein, the monocrystalline silicon piece is 110 crystal faces or 221 crystal faces away from the surface of the crucible bottom.
Wherein, the default spacing between the two neighboring monocrystalline silicon piece is not more than 20mm.
Wherein, the default spacing between the two neighboring monocrystalline silicon piece is 2~5mm.
Wherein, the default spacing includes the first default spacing and the second default spacing, and the first default spacing is greater than
Second default spacing, wherein the first default spacing is 110 adjacent crystal faces of the two neighboring monocrystalline silicon piece and 221 crystal faces
Side between spacing, the second default spacing is adjacent non-110 crystal face or non-221 of the two neighboring monocrystalline silicon piece
Spacing between the side of crystal face.
Wherein, the monocrystalline silicon piece has opposite first surface and second surface, and the first surface is plane, puts
It sets in the bottom of the crucible；
The second surface is plane, or, the second surface is partial cylinder side；
Height of the second surface of each monocrystalline silicon piece in the crucible is identical.
Wherein, the monocrystalline silicon piece with a thickness of 10mm~25mm.
Wherein, the place mat polycrystalline particle at the default spacing includes：
Place mat diameter is less than the polycrystalline particle of 2mm at the default spacing.
Polycrystalline silicon ingot casting method provided by the present invention, in multiple monocrystalline silicon pieces in the place mat of array distribution in crucible bottom
When, prepsetting gap is reserved between adjacent single crystalline silicon wafer, after being laid with and completing monocrystalline silicon piece, by place mat polysilicon in default spacing
Particle, so that polycrysalline silcon and monocrystalline silicon piece are collectively as seed crystal.During ingot casting, after fusing, silicon liquid parent phase
Basic to solve the induction of silicon liquid crystal orientation in monocrystalline silicon piece crystal face epitaxial growth, single-crystal platy seed crystal face passes through epitaxial growth regime
Monocrystalline consistent with single-crystal lattice is grown, little particle seed edge bevel surface homogeneous nucleation grows high-efficiency polycrystalline；Due to monocrystalline dislocation
Low, monocrystalline silicon sheet surface epitaxial growth crystal inherits monocrystalline low dislocation feature, fundamentally reduces crystal bottom dislocation etching pits, from
And reach fast lifting silicon wafer transformation efficiency result.
In order to further promote the low dislocation of polycrystalline cast ingot and the effect of high transformation efficiency, of the invention another specific
In embodiment, also further using 110 crystal faces of monocrystalline silicon piece or 221 crystal faces as the surface for deviating from crucible bottom, then singly
110 crystal faces or 221 crystal faces of crystal silicon chip are the preferred growth face of monocrystalline silicon piece, can effectively control monocrystalline silicon piece and polycrystalline
Grain intersection stress generates, and crystal growth region area and low defect can be effectively maintained, thus Improving The Quality of Products.
In conclusion polycrystalline silicon ingot casting method provided by the present invention, can largely reduce dislocation defects
Problem, and the finished product conversion ratio of polysilicon is improved, the polycrystal silicon ingot of more high yield quality is obtained, and then improve polysilicon production
The performance of product.
Detailed description of the invention
It, below will be to embodiment or existing for the clearer technical solution for illustrating the embodiment of the present invention or the prior art
Attached drawing needed in technical description is briefly described, it should be apparent that, the accompanying drawings in the following description is only this hair
Bright some embodiments for those of ordinary skill in the art without creative efforts, can be with root
Other attached drawings are obtained according to these attached drawings.
Fig. 1 is the flow diagram of polycrystalline silicon ingot casting method provided by the embodiment of the present invention；
Fig. 2 is the schematic diagram of crucible bottom seed crystal place mat provided in an embodiment of the present invention；
Fig. 3 is the structural schematic diagram of the monocrystalline silicon piece provided in the embodiment of the present invention；
Fig. 4 is the structural schematic diagram of another monocrystalline silicon piece provided in an embodiment of the present invention.
Specific embodiment
Partly melt in technique in polycrystalline silicon ingot casting, generallys use polycrystalline fine particle silicon or fragment place mat crucible bottom as seed
Crystalline substance, heating, fusing, fusing later period make crucible bottom seed crystal non-fusible by controlling heat-insulation cage aperture, quickly jump into long brilliant rank
Duan Hou, by reducing TC1 temperature and promoting heat-insulation cage, silicon liquid parent phase is grown in seed crystal face fast nucleation, but growth course
In due to the competitive relation between crystal grain, lead to the generation of a large amount of stress between crystal boundary and crystal boundary, thus cause dislocation defects quick
Increment.
Also have and crucible bottom be laid on as seed crystal using monocrystalline block, but during monocrystalline block place mat monocrystalline block with
Monocrystalline block must assure that seamless, since the crystal boundary of monocrystalline and monocrystalline has a large amount of stress during the growth process, thus cause
Edge joint position generates a large amount of low-angle boundary, and low-angle boundary quickly causes crystal quality to be difficult to ensure to horizontal proliferation, thus
Cause quasi- monocrystalline crystal forming rate low.
By being optimized to seed crystal in the present invention, will fundamentally be reduced brilliant using monocrystalline silicon piece used as seed crystal
Body bottom dislocation etching pits, to reach fast lifting silicon wafer transformation efficiency result.
In order to enable those skilled in the art to better understand the solution of the present invention, with reference to the accompanying drawings and detailed description
The present invention is described in further detail.Obviously, described embodiments are only a part of the embodiments of the present invention, rather than
Whole embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making creative work premise
Under every other embodiment obtained, shall fall within the protection scope of the present invention.
As shown in FIG. 1, FIG. 1 is the flow diagram of polycrystalline silicon ingot casting method provided by the embodiment of the present invention, this method
May include：
Step S1：Multiple monocrystalline silicon pieces being arranged in array are laid in crucible bottom, are had between adjacent single crystalline silicon wafer pre-
If spacing.
Step S2：Polycrysalline silcon is filled in default spacing.
Specifically, it can refer to Fig. 2, Fig. 2 is the schematic diagram of crucible bottom seed crystal place mat provided in an embodiment of the present invention.Fig. 2
In monocrystalline silicon piece 1 be arranged in array in crucible bottom, and polycrystalline particle 2 is being distributed between monocrystalline silicon piece 1.
It should be noted that monocrystalline block used in the prior art as seed crystal place mat crucible bottom scheme
In, it needs to be bonded laying between monocrystalline block, to keep completely seamless between monocrystalline block and monocrystalline block, technique is wanted
Seeking Truth is very high, once the gap between monocrystalline block can not be bonded, between monocrystalline block side during the growth process
There may be stress, edge joint position is thus caused to generate low-angle boundary, low-angle boundary quickly leads to crystal to horizontal proliferation
Quality is difficult to ensure, thus causes crystal forming rate low.
Therefore, in the present embodiment, polycrysalline silcon and monocrystalline silicon piece are collectively as seed crystal.After fusing terminates to jump,
Single-crystal platy seed crystal face grows monocrystalline consistent with single-crystal lattice by epitaxial growth regime, little particle seed crystal face homogeneity at
Nucleus growth goes out high-efficiency polycrystalline, so that small silico briquette monocrystalline area is greater than 80% after crystal ingot evolution, the crystal in monocrystalline area is due to length
The holding of crystal region low dislocation feature during crystalline substance, relatively common high-efficiency polycrystalline defect reduce by 45% or more, and efficiency effectively mentions
Rise 0.15-0.3%.
Step S3：Silicon material is placed on monocrystalline silicon piece, crucible is heated, and makes melting silicon materials.
Step S4：After all melting silicon materials, stop heating, the silicon material for controlling molten condition is nucleated in monocrystalline silicon sheet surface
Growth forms polycrystal silicon ingot.
Specifically, technique, including loading stage are partly melted using polycrystalline silicon ingot casting in the present embodiment：It is laid in crucible bottom
The thickness of one layer of monocrystalline silicon piece, thickness and monocrystalline silicon piece is equal, in other words, the monocrystalline silicon of single layer is only laid in crucible bottom
Piece is laid with polycrystalline silicon material without stacking monocrystalline silicon piece, then in the gap between monocrystalline silicon piece, is laid with the thickness of polycrystalline silicon material
Degree is approximately equal with the thickness of monocrystalline silicon piece, and the spacing between monocrystalline silicon piece is filled up；After the completion of laying, then in monocrystalline silicon
Piece stacked on top places silicon material, specifically can be using purity in the silicon material of 5.5N~6.5N, and the amount of silicon material is generally according to crucible ruler
Very little setting, usually in 800Kg~900Kg.
Melting stage：After the completion of loading stage, it the inert gases conduct such as can will vacuumize, or be filled with argon gas in ingot furnace
Protective gas；The silicon material in crucible is heated from the side of crucible and top by the heating device in ingot furnace again, is made
It obtains temperature and is promoted to 1000 DEG C or more in 1h~2h, until the melting silicon materials in crucible, heat-insulation cage is constantly in closing at this time
State, aperture 0 melt the later period, within 4h~8h, slowly promote the height of heat-insulation cage, control heat-insulation cage aperture is mentioned by 0cm
7cm degree or so is risen to, so that crucible bottom is rapidly cooled, melting silicon materials and crucible bottom portion of monocrystalline silicon inside final crucible
Piece is non-fusible.
Crystal growing stage：After silicon material thawing, after quickly jumping into crystal growing stage, by reducing TC1 temperature and promoting heat-insulation cage,
Heat-insulation cage aperture is promoted to 20cm by 7cm, silicon liquid parent phase is grown in monocrystalline silicon sheet surface fast nucleation, ultimately generates polysilicon
Ingot.
It should be noted that in the prior art there is also as seed crystal being layed in crucible bottom using monocrystalline block, but
It is to require to be fitted close between monocrystalline block.And in the actual operation process, it have been kept between monocrystalline block and monocrystalline block
Completely without gap, the requirement to technique is very high, once the gap between monocrystalline silicon material can not be bonded, monocrystalline silicon material side
There may be stress between face during the growth process, edge joint position is thus caused to generate low-angle boundary, low-angle boundary is quick
Cause crystal quality to be difficult to ensure to horizontal proliferation, thus causes crystal forming rate low.
Using technique is partly melted in the present invention, by being optimized to seed crystal, match relative to by monocrystalline silicon piece and polycrystalline particle
It closes used as seed crystal, without being bonded to each other between monocrystalline silicon piece, reduces the technology difficulty of seed crystal laying.And in ingot casting mistake
Cheng Zhong, after fusing, silicon liquid parent phase is induced in monocrystalline silicon piece crystal face epitaxial growth, the basic silicon liquid crystal orientation that solves, single-chip
Shape seed crystal face grows monocrystalline consistent with single-crystal lattice by epitaxial growth regime, and little particle seed edge bevel surface homogeneous nucleation is raw
Grow high-efficiency polycrystalline；Since monocrystalline dislocation is low, monocrystalline silicon sheet surface epitaxial growth crystal inherits monocrystalline low dislocation feature, from basic
Upper reduction crystal bottom dislocation etching pits, to reach fast lifting silicon wafer transformation efficiency result.
Optionally, in another embodiment of the present invention, can also further include：
Monocrystalline silicon piece is 110 crystal faces or 221 crystal faces away from the surface of crucible bottom.
It should be noted that the aufwuchsplate of seed crystal is frequently with 100 during the polycrystalline cast ingot of conventional pulling of crystals seeding
Crystal face or 111 crystal faces.110 crystal face of monocrystalline silicon piece preferred growth face or 221 crystal faces are used in the present embodiment, due to preferred growth face
Crystal orientation direction of growth feature, form a special grain boundary in monocrystalline silicon piece and polycrystalline particle intersection, special grain boundary can have
Effect slows down monocrystalline silicon piece and polycrystalline particle intersection crystal grain stress generates, and avoids poly grains from expanding to monocrystalline silicon piece region, energy
Monocrystalline silicon piece growth district area and low defect are effectively maintained, thus Improving The Quality of Products.
Based on the above embodiment, in another embodiment of the present invention, can further include：
Between the monocrystalline silicon piece that crucible bottom is laid with, the default spacing between adjacent single crystalline silicon wafer, which is greater than, is not more than 20mm.
Preferably, the default spacing between two neighboring monocrystalline silicon piece is 2~5mm.
It should be noted that the polycrystal silicon ingot to be produced in the present invention is the silicon ingot of class monocrystalline, although belonging to polycrystalline model
Farmland, but its crystal phase structure is regular distribution in a small range.
When the spacing between adjacent single crystalline silicon wafer is excessive, then it will lead to the reduction of monocrystalline silicon piece seeding area, very big
The irregular polycrystalline of crystal phase structure can be grown in the gap between monocrystalline silicon piece in degree, influence the quality of class monocrystalline.Cause
This, the distance in the present embodiment between monocrystalline silicon piece specifically should can be 2mm, 5mm, 10mm, 15mm, 20mm no more than 20mm
Deng.
But when the spacing between monocrystalline silicon piece is too small, it is possible to generate at the gap between monocrystalline silicon piece a large amount of
Low-angle boundary, cause crystal ingot to be scrapped, therefore, more preferably embodiment in the present invention, being will be between monocrystalline silicon piece
Spacing is arranged in 2mm~5mm.
Optionally, in another embodiment of the present invention, can further include：
Default spacing includes the first default spacing and the second default spacing, and the first default spacing is greater than the second default spacing,
Wherein spacing of the first default spacing between the side of two neighboring monocrystalline silicon piece adjacent 110 crystal faces or 221 crystal faces, second
Default spacing is the spacing between adjacent non-110 crystal face of two neighboring monocrystalline silicon piece and the side of non-221 crystal face.
It should be noted that can either can also be made in the present invention using 110 crystal faces as preferred growth face with 221 crystal faces
For preferred growth face.So, when using 221 crystal faces as first aufwuchsplate, there may also be the crystal faces of a side for monocrystalline silicon piece
For 110 faces.Therefore, the side between adjacent monocrystalline silicon piece can be divided into the side of 110 crystal faces or 221 crystal faces and non-110 brilliant
Face and the side of non-221 crystal face.
For the side of adjacent 110 crystal faces or 221 crystal faces, due to its special crystal phase, two adjacent sides
Between spacing can be set it is relatively large；Conversely, between the side of adjacent non-110 crystal face and non-221 crystal face
Spacing then should be small as far as possible.
As previously mentioned, the monocrystalline silicon piece in the present invention is obtained by cutting silicon single crystal rod, and currently used list
Crystalline silicon rod is usually the silicon rod of cuboid or the silicon rod of cylindrical body.
Therefore, in another embodiment of the present invention, can also further include：
Monocrystalline silicon piece has opposite first surface and second surface, and first surface is plane, is placed on the bottom of crucible
Portion；
Second surface specifically can refer to Fig. 3 for plane, and the first surface and second surface of the monocrystalline silicon piece are equal
For rectangle, which can be slab construction.
Second surface can also be partial cylinder side, as shown in figure 4, second surface can be semicolumn side, the list
Crystal silicon chip can be part cylindrical, but cylindrical side is the second surface away from crucible bottom.
In addition, no matter what shape the second surface of monocrystalline silicon piece is, the thickness of each monocrystalline silicon piece should be all the same,
It is that height of the second surface height of each monocrystalline silicon piece in crucible is all the same.
It should be noted that the monocrystalline silicon piece of other shapes structure is not precluded in the present invention, as long as with crucible ground phase
The face of fitting is plane.But more Preferable scheme is that using regular shape monocrystalline silicon piece, Edge position control monocrystalline silicon
Reserved spacing between piece.In addition, since current conventional silicon rod is substantially cylindrical body or cuboid, then, for upper and lower
Surface is rectangle plane, and the silicon wafer being parallel to each other directly can be obtained by the silicon rod axial slices to cuboid, and right
For the monocrystalline silicon piece with semi-cylindrical, it can also be obtained and circumferentially cutting to cylindrical type silicon rod, so rectangular surfaces
Monocrystalline silicon piece and semi-cylindrical monocrystalline silicon piece it is most readily available, can reduce the cutting difficulty of single silicon wafer.
Optionally, for the size of monocrystalline silicon piece, by taking rectangular plate structure as an example, length can in 200mm~1000mm,
Width can be in 100mm~300mm.
Optionally, the thickness of single silicon wafer can be 10cm~25cm, specifically, can be 10cm, 12cm, 15cm,
17cm、20cm、23cm、25cm。
Further, in another embodiment of the present invention, it is laid at the default spacing between monocrystalline silicon piece
Polycrysalline silcon can specifically be less than the polycrystalline particle of 2mm using diameter.
As previously described it is found that the diameter of polycrystalline particle is much smaller than the thickness of monocrystalline silicon piece, and it is less than between monocrystalline silicon piece
Reserved spacing, then polycrystalline particle can be more fully filled between monocrystalline silicon piece.
Each embodiment in this specification is described in a progressive manner, the highlights of each of the examples are with it is other
The difference of embodiment, same or similar part may refer to each other between each embodiment.
Polycrystalline silicon ingot casting method provided by the present invention is described in detail above.Specific case used herein
Principle and implementation of the present invention are described, the above embodiments are only used to help understand side of the invention
Method and its core concept.It should be pointed out that for those skilled in the art, not departing from the principle of the invention
Under the premise of, it can be with several improvements and modifications are made to the present invention, these improvement and modification also fall into the claims in the present invention
In protection scope.
Claims (8)
1. a kind of polycrystalline silicon ingot casting method, which is characterized in that including：
Multiple monocrystalline silicon pieces being arranged in array are laid in crucible bottom, there is default spacing between the adjacent monocrystalline silicon piece；
Polycrysalline silcon is filled in the default spacing；
Silicon material is placed on the monocrystalline silicon piece, the crucible is heated, makes the melting silicon materials；
After all melting silicon materials, stop heating, control the silicon material of molten condition the monocrystalline silicon sheet surface at
Nucleus growth forms polycrystal silicon ingot.
2. polycrystalline silicon ingot casting method according to claim 1, which is characterized in that the monocrystalline silicon piece deviates from the crucible bottom
The surface in portion is 110 crystal faces or 221 crystal faces.
3. polycrystalline silicon ingot casting method according to claim 2, which is characterized in that between the two neighboring monocrystalline silicon piece
The default spacing is not more than 20mm.
4. polycrystalline silicon ingot casting method according to claim 3, which is characterized in that between the two neighboring monocrystalline silicon piece
The default spacing is 2~5mm.
5. polycrystalline silicon ingot casting method according to claim 3, which is characterized in that the default spacing includes between first default
Away from the second default spacing, the first default spacing be greater than the second default spacing, wherein the first default spacing be it is adjacent
Spacing between 110 adjacent crystal faces of two monocrystalline silicon pieces and the side of 221 crystal faces, the second default spacing are adjacent
Spacing between adjacent non-110 crystal face of two monocrystalline silicon pieces or the side of non-221 crystal face.
6. polycrystalline silicon ingot casting method according to any one of claims 1 to 5, which is characterized in that the monocrystalline silicon piece has
Opposite first surface and second surface, the first surface are plane, are placed on the bottom of the crucible；
The second surface is plane, or, the second surface is partial cylinder side；
Height of the second surface of each monocrystalline silicon piece in the crucible is identical.
7. polycrystalline silicon ingot casting method according to claim 6, which is characterized in that the monocrystalline silicon piece with a thickness of 10mm~
25mm。
8. polycrystalline silicon ingot casting method according to claim 6, which is characterized in that the place mat at the default spacing is more
Brilliant particle includes：
Place mat diameter is less than the polycrystalline particle of 2mm at the default spacing.
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