CN109306518A - A kind of growing silicon ingot/crystal bar crucible and preparation method thereof - Google Patents
A kind of growing silicon ingot/crystal bar crucible and preparation method thereof Download PDFInfo
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- CN109306518A CN109306518A CN201811509794.9A CN201811509794A CN109306518A CN 109306518 A CN109306518 A CN 109306518A CN 201811509794 A CN201811509794 A CN 201811509794A CN 109306518 A CN109306518 A CN 109306518A
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- Prior art keywords
- crucible
- coating
- barium hydroxide
- silicon nitride
- silicon
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 55
- 239000010703 silicon Substances 0.000 title claims abstract description 55
- 239000013078 crystal Substances 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000011248 coating agent Substances 0.000 claims abstract description 76
- 238000000576 coating method Methods 0.000 claims abstract description 76
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 54
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 claims abstract description 48
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 47
- 229910001863 barium hydroxide Inorganic materials 0.000 claims abstract description 47
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 47
- 150000001875 compounds Chemical class 0.000 claims abstract description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 109
- 239000000377 silicon dioxide Substances 0.000 claims description 57
- 239000007788 liquid Substances 0.000 claims description 41
- 230000000873 masking effect Effects 0.000 claims description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 229910001868 water Inorganic materials 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 8
- 229910002804 graphite Inorganic materials 0.000 claims description 8
- 239000010439 graphite Substances 0.000 claims description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- XJKVPKYVPCWHFO-UHFFFAOYSA-N silicon;hydrate Chemical compound O.[Si] XJKVPKYVPCWHFO-UHFFFAOYSA-N 0.000 claims description 3
- 239000004408 titanium dioxide Substances 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 abstract description 51
- 238000000034 method Methods 0.000 abstract description 26
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 230000015572 biosynthetic process Effects 0.000 abstract description 5
- 239000002131 composite material Substances 0.000 abstract description 5
- 150000004767 nitrides Chemical class 0.000 abstract description 3
- 230000000694 effects Effects 0.000 description 9
- 239000002210 silicon-based material Substances 0.000 description 9
- 238000005266 casting Methods 0.000 description 8
- 238000002955 isolation Methods 0.000 description 8
- 229910052681 coesite Inorganic materials 0.000 description 7
- 229910052906 cristobalite Inorganic materials 0.000 description 7
- 229910052682 stishovite Inorganic materials 0.000 description 7
- 229910052905 tridymite Inorganic materials 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 3
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Inorganic materials [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910003978 SiClx Inorganic materials 0.000 description 2
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000008199 coating composition Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 229910052571 earthenware Inorganic materials 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- -1 hydrogen Barium monoxide Chemical class 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 239000011344 liquid material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000010257 thawing Methods 0.000 description 2
- 241000790917 Dioxys <bee> Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- CSSYLTMKCUORDA-UHFFFAOYSA-N barium(2+);oxygen(2-) Chemical compound [O-2].[Ba+2] CSSYLTMKCUORDA-UHFFFAOYSA-N 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
Classifications
-
- 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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/10—Crucibles or containers for supporting the melt
-
- 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
- C30B28/06—Production of homogeneous polycrystalline material with defined structure from liquids by normal freezing or freezing under temperature gradient
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The present invention provides a kind of growing silicon ingot/crystal bar crucibles and preparation method thereof.Crucible provided by the invention includes crucible body and the coating for being compound in the crucible body outer surface；The coating is silicon nitride coating or barium hydroxide coating.The present invention is in crucible body outer surface composite nitride silicon coating or barium hydroxide coating, it is physically or chemically reacted by this layer of coating to completely cut off crucible and backplate/crucible support, to reduce silicon ingot/crystal bar carbon content, avoid because carbon content it is exceeded caused by a large amount of traditional methods of indicating the pronunciation of a Chinese character, the Hard Inclusion for also avoiding high-carbon content formation keeps slice link more smooth, reduces residual rate of breaking, influence of the stria to slicing processes and yield is largely reduced, production cost is reduced.
Description
Technical field
The present invention relates to crucible technique field, in particular to a kind of growing silicon ingot/crystal bar crucible and preparation method thereof.
Background technique
In pulling of crystals and polycrystalline cast ingot, crucible is most important, provides a package silicon material and growth ingot casting/crystal bar
Place.Specifically, silicon material is placed in crucible, it is (right or for graphite crucible or crucible support that crucible periphery is enclosed with graphite protective plate
Crucible plays support protective effect), silicon material carries out high-temperature process in crucible, through silicon liquid thawing and crystal growing process, forms silicon
Ingot/crystal bar.
Currently, China's growing silicon ingot/crystal bar is quartz-ceramics material with crucible, main component is silica.It is existing
SiO during ingot casting and crystal pulling, under high temperature, in crucible2Following reaction: C+SiO can occur with the C ingredient in graphite crucible support2=
CO+SiO, generated CO can be entered in the silicon liquid contained in crucible and be formed carbon impurity, lead to the carbon in gained silicon ingot/crystal bar
Content increases.And high carbon content can be such that the exceeded traditional method of indicating the pronunciation of a Chinese character of a large amount of carbon of crystal formation scraps, and increase significantly drawing cost；High
Carbon content can also make to form Hard Inclusion and impurity shade inside polycrystalline, reduce crystal forming rate, and Hard Inclusion also will cause slice stria, sternly
Slice broken string is also resulted in if weight to scrap.Therefore, the carbon content for controlling and reducing in silicon ingot/crystal bar is of great significance.
Summary of the invention
In view of this, the present invention provides a kind of growing silicon ingot/crystal bar crucibles and preparation method thereof, using of the invention
Crucible can reduce silicon ingot/crystal bar phosphorus content, and then a large amount of traditional methods of indicating the pronunciation of a Chinese character and the shape of Hard Inclusion caused by avoiding carbon content exceeded
At it is more smooth to make to be sliced link, reduces breakage ratio, largely reduces influence of the stria to slicing processes and yield, and then reduces
Silicon ingot/crystal bar production cost.
The present invention provides a kind of growing silicon ingot/crystal bar crucible, including crucible body and it is compound in the crucible body
The coating of outer surface；
The coating is silicon nitride coating or barium hydroxide coating.
It preferably, include silicon nitride and silica in the silicon nitride coating；It include hydrogen in the barium hydroxide coating
Barium monoxide and silica.
Preferably, the mass ratio of silicon nitride and silica is (1~1.2) in the silicon nitride coating: (1.4~
1.65)；
In the barium hydroxide coating, the mass ratio of barium hydroxide and silica is (20~25): (28~35).
Preferably, the coating with a thickness of 1~2.5mm.
Preferably, the wall thickness of the crucible body is 8~13mm, and diameter is 980~1070mm.
Preferably, the crucible body is silica crucible.
Preferably, the crucible periphery is provided with crucible support.
Preferably, the crucible support is graphite crucible support.
The present invention also provides a kind of preparation method of growing silicon ingot as described in the above technical scheme/crystal bar crucible,
Include:
Masking liquid and drying are coated in crucible body outer surface, obtains growing silicon ingot/crystal bar crucible；
The masking liquid is silicon nitride masking liquid or barium hydroxide masking liquid.
Preferably, it is (4~5): (16~18) that the silicon nitride masking liquid, which includes mass ratio: the silicon nitride of (4~5), water and
Silica solution；
The barium hydroxide masking liquid includes that mass ratio is (1.0~1.4): (2.5~2.9): the hydroxide of (0.8~1.2)
Barium, water and silica solution；
The temperature of the drying is 90~110 DEG C, and the time is 30~60min.
The present invention provides a kind of growing silicon ingot/crystal bar crucible, in crucible body outer surface composite nitride silicon coating or
Barium hydroxide coating is physically or chemically reacted by this layer of coating to completely cut off crucible and backplate/crucible support, thus reduce silicon ingot/
The carbon content of crystal bar, avoid because carbon content it is exceeded caused by a large amount of traditional methods of indicating the pronunciation of a Chinese character, it is thus also avoided that high-carbon content formed Hard Inclusion, make
It is more smooth to be sliced link, reduces residual rate of breaking, largely reduces influence of the stria to slicing processes and yield, reduces production cost,
Improve the competitiveness of Products.
The experimental results showed that compared to common crucible, it, can be by silicon ingot/crystal bar product drop using crucible of the invention
Carbon amounts > 2ppm, this in actual production, can effectively avoid because carbon content it is exceeded caused by a large amount of traditional methods of indicating the pronunciation of a Chinese character, it is thus also avoided that high-carbon
The Hard Inclusion that content is formed, makes to be sliced that link is more smooth, and reduction is broken residual rate, largely reduces stria to slicing processes and yield
It influences, reduces company cost.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
The embodiment of invention for those of ordinary skill in the art without creative efforts, can also basis
The attached drawing of offer obtains other attached drawings.
Fig. 1 is the schematic diagram for the polycrystalline crucible that one embodiment of the present of invention provides；
Fig. 2 is the schematic diagram for the single crystal crucible that one embodiment of the present of invention provides.
Specific embodiment
The present invention provides a kind of growing silicon ingot/crystal bar crucible, including crucible body and it is compound in the crucible body
The coating of outer surface；
The coating is silicon nitride coating or barium hydroxide coating.
Referring to Fig. 1, Fig. 1 is the schematic diagram for the polycrystalline crucible that one embodiment of the present of invention provides, wherein 1 is crucible sheet
Body, 2 be coating.
Crucible body 1 is for containing silicon liquid/silicon material, growing silicon ingot or crystal bar, specifically, silicon liquid/silicon material carries out in crucible
High-temperature process forms polycrystal silicon ingot/monocrystalline crystal bar through silicon liquid thawing and crystal growing process.
In one embodiment of the invention, crucible body 1 is silica crucible.
The present invention is not particularly limited the shape of crucible body 1, is common crucible class well known to those skilled in the art
Type；In some embodiments of the invention, crucible body 1 is cylindrical crucible, conical crucible, arc crucible or saggar
Crucible.Referring to Fig. 1, for the polycrystalline crucible schematic diagram that one embodiment of the present of invention provides, crucible body is rectangle crucible.
Referring to fig. 2, Fig. 2 is the schematic diagram for the single crystal crucible that one embodiment of the present of invention provides, and crucible body therein is arc earthenware
Crucible.
The present invention is not particularly limited the size of crucible body 1, to be well known to those skilled in the art for growing list
The crucible size of crystal silicon or polysilicon.In some embodiments of the invention, the wall thickness of crucible body 1 is 8~13mm, directly
Diameter is 980~1070mm.In the present invention, " diameter " is maximum gauge, for the crucible inconsistent for upper and lower shape, earthenware
Diameter is different up and down for crucible ontology, and " diameter " is the maximum gauge in crucible body.In the present invention, " diameter " is outer
Diameter.
Coating 2 is compound in the outer surface of crucible body 1, and crucible body is isolated from the outside world.
In one embodiment of the invention, coating 2 is silicon nitride coating；Silicon nitride coating can be by crucible body and crucible
The backplate of periphery/crucible support isolation is opened, and crucible body is avoided directly to contact with backplate/crucible support, and following reaction: C+ occurs at high temperature
SiO2=CO+SiO, and then avoid CO and enter in the silicon liquid contained in crucible, silicon ingot/crystal bar product carbon content is reduced,
And then the formation of a large amount of traditional methods of indicating the pronunciation of a Chinese character and Hard Inclusion caused by avoiding carbon content exceeded, keep slice link more smooth, reduces broken string
Rate largely reduces influence of the stria to slicing processes and yield, and then reduces silicon ingot/crystal bar production cost, and it is competing to promote product
Strive power.
In the present invention, the silicon nitride coating preferably comprises silicon nitride and silica, by silicon nitride and silica
Mixture could completely cut off backplate/crucible support of crucible body Yu crucible periphery as coating, reduce product carbon content.In the present invention,
In the silicon nitride coating, the mass ratio of silicon nitride and silica is preferably (1~1.2): (1.4~1.65)；In the present invention
Some embodiments in, in silicon nitride coating, the mass ratio of silicon nitride and silica is 1: 1.2.If silicon nitride content is too low
Or it is excessively high, then cannot effectively completely cut off backplate reacted with crucible body generate CO enter in the silicon liquid in crucible, product carbon drop effect
Fruit is obviously deteriorated, and silicon ingot/crystal bar product carbon content cannot be effectively reduced.
The present invention is not particularly limited the preparation method of silicon nitride coating, is coating system well known to those skilled in the art
Standby mode, such as can brush or spray to the outer surface of crucible body 1 by silicon nitride masking liquid.In the present invention, the silicon nitride
Masking liquid is preferably the mixed liquor of silicon nitride, silica solution and water, using the mixed liquor as masking liquid, can either preferably be adhered to crucible
Outer surface, and the coating with effectively isolation effect can be formed.In some embodiments, the silicon nitride, water and silica solution
Mass ratio is (4~5): (16~18): (4~5).The present invention is not particularly limited the concentration of the silica solution, for conventional city
Sell commodity；In some embodiments, the silica solution is SiO2Content is the silica solution of 20wt%~30wt%.
In another embodiment of the present invention, coating 2 is barium hydroxide coating；Carrying out high growth temperature silicon ingot/crystal bar
When, it is other in furnace to generate carbon dioxide gas, the titanium dioxide containing carbon parts (such as calandria, backplate and other thermal field materials)
Carbon gas penetrates into barium hydroxide coating, reacts as follows with the barium hydroxide generation in coating: Ba (OH)2+CO2=BaCO3+
H2O, the BaCO of generation3Excellent insulating effect is played to crucible body, by backplate/crucible support of crucible body and crucible periphery every
It opens absolutely, avoids the two directly contact from reacting, generate CO, and then avoid CO and enter in the silicon liquid contained in crucible, reduction
Silicon ingot/crystal bar product carbon content, and then the formation of a large amount of traditional methods of indicating the pronunciation of a Chinese character and Hard Inclusion caused by avoiding carbon content exceeded, make
It is more smooth to be sliced link, reduces breakage ratio, largely reduces influence of the stria to slicing processes and yield, so reduce silicon ingot/
The production cost of crystal bar.
In the present invention, the barium hydroxide coating preferably includes barium hydroxide and silica, by barium hydroxide and dioxy
The mixture of SiClx could completely cut off backplate/crucible support of crucible body Yu crucible periphery as coating, reduce product carbon content.This hair
In bright, in the barium hydroxide coating, the mass ratio of barium hydroxide and silica is preferably (20~25): (28~35)；?
In some embodiments of the present invention, in barium hydroxide coating, the mass ratio 1: 1.2 of barium hydroxide and silica.If hydroxide
Barium content is too low or excessively high, then cannot effectively completely cut off backplate reacted with crucible body generate CO enter in the silicon liquid in crucible,
Product carbon drop effect is obviously deteriorated, and silicon ingot/crystal bar product carbon content cannot be effectively reduced.
The present invention is not particularly limited the preparation method of barium hydroxide coating, is coating well known to those skilled in the art
Barium hydroxide masking liquid can such as be brushed or be sprayed to the outer surface of crucible body 1 by preparation method.In the present invention, the hydrogen
Barium monoxide masking liquid is preferably the mixed liquor of barium hydroxide, silica solution and water, using the mixed liquor as masking liquid, can either preferably be glued
It is attached to crucible outer surface, and the coating with effectively isolation effect can be formed.In some embodiments, the barium hydroxide, water
Mass ratio with silica solution is (1.0~1.4): (2.5~2.9): (0.8~1.2).The present invention does not have the concentration of the silica solution
Have it is specifically limited, be conventional commercial commodity；In some embodiments, the silica solution is SiO2Content be 20wt%~
The silica solution of 30wt%.
In some embodiments of the invention, coating 2 with a thickness of 1~2.5mm.It, can when practical brushing or spray-on coating
The coating of different-thickness is obtained by controlling the round-trip number of spray gun.
In one embodiment of the invention, crucible periphery is additionally provided with crucible support.Referring to Fig. 1, wherein 3 be crucible support.Coating
2 open crucible body 1 and the isolation of crucible support 3, avoid the two directly contact.
In one embodiment of the invention, crucible support 3 is graphite crucible support.
The present invention provides a kind of growing silicon ingot/crystal bar crucible, in crucible body outer surface composite nitride silicon coating or
Barium hydroxide coating is physically or chemically reacted by this layer of coating to completely cut off crucible and backplate/crucible support, thus reduce silicon ingot/
The carbon content of crystal bar, avoid because carbon content it is exceeded caused by a large amount of traditional methods of indicating the pronunciation of a Chinese character, it is thus also avoided that high-carbon content formed Hard Inclusion, make
It is more smooth to be sliced link, reduces residual rate of breaking, largely reduces influence of the stria to slicing processes and yield, reduces company cost,
Improve the competitiveness of Products.The experimental results showed that compared to the conventional crucible of non-composite coating, crucible of the invention,
Silicon ingot/crystal bar product carbon content can be made to reduce 2ppm or more, be of great significance to actual production.
The present invention also provides a kind of preparation method of growing silicon ingot as described in the above technical scheme/crystal bar crucible,
Include:
Masking liquid and drying are coated in crucible body outer surface, obtains growing silicon ingot/crystal bar crucible；
The masking liquid is silicon nitride masking liquid or barium hydroxide masking liquid.
In the present invention, the silicon nitride masking liquid is preferably the mixed liquor of silicon nitride, silica solution and water, using the mixed liquor as
Masking liquid can either preferably be adhered to crucible outer surface, and can form the coating with effectively isolation effect.Preferably, described
The mass ratio of silicon nitride, water and silica solution is (4~5): (16~18): (4~5).The present invention does not have the concentration of the silica solution
Have it is specifically limited, be conventional commercial commodity；In some embodiments, the silica solution is SiO2Content be 20wt%~
The silica solution of 30wt%.
In the present invention, the barium hydroxide masking liquid is preferably the mixed liquor of barium hydroxide, silica solution and water, by the mixed liquor
As masking liquid, it can either be preferably adhered to crucible outer surface, and the coating with effectively isolation effect can be formed.Preferably,
The mass ratio of the barium hydroxide, water and silica solution is (1.0~1.4): (2.5~2.9): (0.8~1.2).The present invention is to institute
The concentration for stating silica solution is not particularly limited, and is conventional commercial commodity；In some embodiments, the silica solution is SiO2
Content is the silica solution of 20wt%~30wt%.
In the present invention, the temperature of the drying is preferably 90~110 DEG C, and the dry time is preferably 30~60min.
The present invention provides a kind of growing silicon ingot/crystal bar crucible preparation methods, coat nitrogen in crucible body outer surface
SiClx masking liquid or barium hydroxide masking liquid and drying are passed through to form silicon nitride coating or barium hydroxide coating by this layer of coating
Physically or chemically reaction, to reduce silicon ingot/crystal bar carbon content, is avoided because of carbon content to completely cut off crucible and backplate/crucible support
A large amount of traditional methods of indicating the pronunciation of a Chinese character caused by exceeded, it is thus also avoided that the Hard Inclusion that high-carbon content is formed keeps slice link more smooth, and reduction is broken residual
Rate largely reduces influence of the stria to slicing processes and yield, reduces company cost, improves the competitiveness of Products.It is real
Test the result shows that, compared to the conventional crucible of non-composite coating, crucible of the invention can be such that silicon ingot/crystal bar product carbon contains
Amount reduces 2ppm or more, is of great significance to actual production.
For a further understanding of the present invention, the preferred embodiment of the invention is described below with reference to embodiment, still
It should be appreciated that these descriptions are only further explanation the features and advantages of the present invention, rather than to the claims in the present invention
Limitation.In following embodiment, material used is commercially available product, wherein and silicon material is polycrystalline silicon material, is provided by Xinjiang complete works producer,
Model virgin polycrystalline silicon 1/3/5 material.
Embodiment 1
By 500g silicon nitride, 1700g water and 500g silica solution (SiO2Content is 25wt%) it is uniformly mixed, obtain silicon nitride
Masking liquid.In silica crucible (wall thickness 10mm, outer diameter 1000mm) outer surface spraying silicon nitride masking liquid and the drying at 100 DEG C
40min, formed 2mm thickness coating (coating composition be silicon nitride and silica, silicon nitride: the mass ratio of silica be 1:
1.2)。
880kg silicon material is packed into crucible, and graphite crucible backplate is fixed on crucible outer surface (referring to Fig. 1), then
It moves into and carries out ingot casting in furnace, 80 hours a length of when maximum temperature is 1480 DEG C, ingot casting in furnace, after the completion of ingot casting, furnace cooling is taken
Sample out.
The print for taking silicon ingot head-tail respectively, using Fourier's infrared tester (model matches silent winged IS50), test is end to end
The carbon content of print, the results show that its head print carbon content is 13ppm.
Embodiment 2
By 1200g barium hydroxide, 2600g water and 900g silica solution (SiO2Content is 25wt%) it is uniformly mixed, obtain hydrogen
Barium monoxide masking liquid.Barium hydroxide masking liquid is sprayed in the silica crucible outer surface (wall thickness 10mm, outer diameter 1000mm) and at 100 DEG C
Dry 40min, forming the coating of 2mm thickness, (coating composition is barium hydroxide and silica, barium hydroxide: the matter of silica
Amount is than being 1: 1.2).
880kg silicon material is packed into crucible, and graphite crucible backplate is fixed on crucible outer surface (referring to Fig. 1), then
It moves into and carries out ingot casting in furnace, 80 hours a length of when maximum temperature is 1480 DEG C, ingot casting in furnace, after the completion of ingot casting, furnace cooling is taken
Sample out.
According to the test mode test product carbon content of embodiment 1, the results show that its head print carbon content is
12.9ppm。
Comparative example 1
It is carried out according to the preparation process of embodiment 1, unlike, used crucible outer surface is not coated by coating.
According to the test mode test product carbon content of embodiment 1, the results show that its head print carbon content is 16ppm.
By the test result of embodiment 1-2 and comparative example 1 it is found that using crucible of the invention, the carbon drop amount of product can be made
> 2ppm, this in actual production, can effectively avoid because carbon content it is exceeded caused by a large amount of traditional methods of indicating the pronunciation of a Chinese character, it is thus also avoided that high-carbon content
The Hard Inclusion of formation keeps slice link more smooth, reduces residual rate of breaking, largely reduce stria to the shadow of slicing processes and yield
It rings, reduces company cost.
Comparative example 2
It is carried out according to the preparation process of embodiment 1, unlike, silicon nitride content is 200g in silicon nitride masking liquid.
According to the test mode test product carbon content of embodiment 1, the results show that its head print carbon content is 16ppm.
Comparative example 3
It is carried out according to the preparation process of embodiment 2, unlike, barium hydroxide content is 200g in barium hydroxide masking liquid.
According to the test mode test product carbon content of embodiment 1, the results show that its head print carbon content is 16ppm.
By the test result of embodiment 1-2 and comparative example 2-3 it is found that the silicon nitride content in silicon nitride coating is too low,
Or barium hydroxide content in barium hydroxide coating it is too low when, the isolation significant effect of coating reduces, the drop of gained silicon ingot product
Carbon effect is obviously deteriorated, with it is uncoated when product carbon content it is suitable, it is seen then that the ingredient in coating is in proportional region of the invention
It is interior to be just able to achieve isolation, product carbon content is effectively reduced.
The above description of the embodiment is only used to help understand the method for the present invention and its core ideas.To these embodiments
A variety of modifications will be readily apparent to those skilled in the art, the general principles defined herein can be with
Without departing from the spirit or scope of the present invention, it realizes in other embodiments.Therefore, the present invention will not be limited
In the embodiments shown herein, and it is to fit to widest model consistent with the principles and novel features disclosed in this article
It encloses.
Claims (10)
1. a kind of growing silicon ingot/crystal bar crucible, which is characterized in that including crucible body and be compound in the crucible body appearance
The coating in face；
The coating is silicon nitride coating or barium hydroxide coating.
2. crucible according to claim 1, which is characterized in that include silicon nitride and titanium dioxide in the silicon nitride coating
Silicon；It include barium hydroxide and silica in the barium hydroxide coating.
3. crucible according to claim 2, which is characterized in that the matter of silicon nitride and silica in the silicon nitride coating
Amount is than being (1~1.2): (1.4~1.65)；
In the barium hydroxide coating, the mass ratio of barium hydroxide and silica is (20~25): (28~35).
4. crucible according to claim 1, which is characterized in that the coating with a thickness of 1~2.5mm.
5. crucible according to claim 1, which is characterized in that the wall thickness of the crucible body is 8~13mm, and diameter is
980~1070mm.
6. crucible according to claim 1, which is characterized in that the crucible body is silica crucible.
7. crucible according to claim 1, which is characterized in that the crucible periphery is provided with crucible support.
8. crucible according to claim 7, which is characterized in that the crucible support is graphite crucible support.
9. a kind of preparation method of growing silicon ingot according to any one of claims 1 to 8/crystal bar crucible, which is characterized in that
Include:
Masking liquid and drying are coated in crucible body outer surface, obtains growing silicon ingot/crystal bar crucible；
The masking liquid is silicon nitride masking liquid or barium hydroxide masking liquid.
10. preparation method according to claim 9, which is characterized in that the silicon nitride masking liquid include mass ratio be (4~
5): (16~18): silicon nitride, water and the silica solution of (4~5)；
The barium hydroxide masking liquid includes that mass ratio is (1.0~1.4): (2.5~2.9): barium hydroxide, the water of (0.8~1.2)
And silica solution；
The temperature of the drying is 90~110 DEG C, and the time is 30~60min.
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Application publication date: 20190205 |