CN108046846B - A kind of casting polysilicon exempts to spray crucible coating layer and preparation method thereof - Google Patents
A kind of casting polysilicon exempts to spray crucible coating layer and preparation method thereof Download PDFInfo
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- 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
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Abstract
The present invention disclose it is a kind of casting polysilicon exempt from spray crucible coating layer and preparation method thereof, the coating successively includes three-layer coating from inside to outside, wherein based on mass percentage, the ingredient of first layer coating includes 4.5~95% silicon oxynitride, 4.5~95% silica and 0.5~5% silica solution；The ingredient of second layer coating includes 5~50% silicon oxynitride, 0.5~50% silica, 0.5~50% silicon nitride, 0.5~5% silica solution and 0.5~5% PVA；The ingredient of third layer coating includes 0.5~95% silicon oxynitride, 0.5~95% silicon nitride, the PAA of 0.5~5% PVA and 0.5~5%.Present invention utilizes silicon oxynitrides both and silicon nitride, and the and feature that silicon oxynitride binding force is strong, it is designed by reasonable ingredient, solve the problems, such as that silicon nitride and sidewall of crucible binding force be not strong, enhance the intensity and compactness of coating, reduce defect and impurity in silicon ingot, help to improve the yield rate of silicon ingot, improves the stability and photoelectric conversion efficiency of photovoltaic module.
Description
Technical field
The present invention relates to the preparation fields of polysilicon casting crucible coating layer, and in particular to a kind of efficient polysilicon casting
With exempt from spray crucible coating layer and preparation method thereof.
Background technique
Photovoltaic is a kind of important green sustainable energy, and casting polysilicon is the most important former material for preparing photovoltaic module
One of material.The fewer higher photoelectric conversion efficiency in order to obtain, impurity and the defect for casting polysilicon the better.Polysilicon is being cast
In the process, generally use high-purity silica crucible as container, but silicon material is in the case where high temperature melting, will and quartz, also
It is that silica reacts, silicon liquid is caused to penetrate into inside crucible, in the case where the coefficient of expansion of quartz and silicon is inconsistent,
The infiltration of silicon liquid may result in crucible rupture, so that the silicon liquid of high temperature flows out, it is possible to cause serious safety accident.Cause
This, to solve this problem, quartz crucible surface is often sprayed one layer of silicon nitride coating.Since silicon nitride is a kind of high temperature resistant
Ceramics, it not only property stablize, the silicon liquid for high temperature of getting along well reacts, and silicon liquid is bad to its wetability so that its
It is not easy infiltration to enter to adhere to crucible, so that ingot casting goes on smoothly and smoothly demoulds.But although by silicon nitride spray finishing
In crucible as release agent, however it remains many problems: first, the impurity inside silica crucible still can be spread at high temperature to be worn
It crosses silicon nitride coating and enters silicon liquid, cause the increase of polycrystalline silicon impurities and defect, reduce the efficiency of photovoltaic module.Second, nitrogen
SiClx itself and silica crucible binding force be not strong, so that silicon nitride is easy to fall in silicon liquid during ingot casting, forms nitridation
Sila particle, silicon nitride inclusions point hardness is very high, not only increases silicon ingot internal flaw, and the photoelectricity for reducing photovoltaic module turns
Efficiency is changed, and be easy to cause diamond wire to break when subsequent Buddha's warrior attendant wire cutting, leads to production accident.Third, nitrogen
The angle of wetting of SiClx itself and silicon liquid is 45 °~50 °, and in the case where angle of wetting is lower than 90 °, solid liquid interface still has wetting
The case where, not only make the nitrogen in silicon nitride diffuse more readily into inside silicon liquid the pollution caused to silicon ingot in this way, but also
It is not smooth or even a possibility that split ingot to increase demoulding, ultimately causes the unstable of Ingot quality.
To solve the above-mentioned problems, the researcher in the industry proposes many schemes.
The Chinese patent of application number 201110281457.0 discloses one kind before spraying silicon nitride, increases in crucible surface
Add containing silica solution~gel glass structure layer, increases the blocking to impurity in this way, but still without solving silicon nitride and two
The not strong problem of silica binding force, the silicon nitride on surface still have the risk polluted in the silicon liquid fallen into.
A kind of barium silicate crystal layer is disclosed application No. is 201620841199.5 Chinese profession and silicon nitride coating is double
The isolation method of layer, barium silicate crystal layer air-tightness is strong, and hardness is high, can prevent impurity inside crucible from expanding by bubble to silicon ingot
It dissipates, reduces pollution of the crucible to silicon ingot.But silicic acid crystal of barium itself contains barium metal, at high temperature, inevitably
The pollution that serious metal ion is caused inside silicon ingot can be largely diffused into.
The researchers such as Xiaoxiao Gong use mixes 3.8wt% nano silica in silicon nitride coating
(Gong X,Du H,Zhang X,et al.Influence of the coating preparation method and of
nanosilica addition on the bonding character of Si3N4,layer on a silica
Crucible [J] .Ceramics International, 2014,40 (5): 7523~7529.), thus increase silicon nitride at
The compactness and intensity of film reduce erosion of the silicon liquid to silicon nitride layer infiltration and to crucible.But the silica of nanometer is not
It is only at high cost, it is not easy to prepare, and be very easy to reunion and micron-sized silicon nitride particle mismatch, it is difficult to uniformly mixing,
It is difficult to reach corresponding effect in large-scale production process.
Summary of the invention
Exempt to spray crucible coating layer and its application the object of the present invention is to provide a kind of casting polysilicon.
Exempt to spray crucible another object of the present invention is to provide a kind of casting polysilicon.
Another object of the present invention is to provide a kind of preparation method for casting polysilicon and exempting from spray crucible.
Technical solution of the present invention specifically:
A kind of casting polysilicon exempts to spray crucible coating layer, which successively includes three-layer coating from inside to outside, wherein pressing quality
Percentage composition meter,
The ingredient of first layer coating includes 4.5~95% silicon oxynitride, 4.5~95% silica and 0.5~5%
Silica solution, in the coating, the sum of all components mass percentage is 100%；
The ingredient of second layer coating includes 5~50% silicon oxynitride, 0.5~50% silica, 0.5~50%
Silicon nitride, 0.5~5% silica solution and 0.5~5% PVA, in the coating, the sum of all components mass percentage is
100%；
The ingredient of third layer coating includes 0.5~95% silicon oxynitride, 0.5~95% silicon nitride, 0.5~5%
The PAA of PVA and 0.5~5%, in the coating, the sum of all components mass percentage is 100%.
As a kind of optimal technical scheme, the ingredient of the first layer coating includes 5~70% silicon oxynitride, 25~
90% silica and 1~5% silica solution；The ingredient of the second layer coating includes 10~50% silicon oxynitride, 5~
40% silica, 5~40% silicon nitride, 1~5% silica solution and 1~5% PVA；The third layer coating at
Divide the silicon oxynitride including 10~35%, 60~85% silicon nitride, the PAA of 1~5% PVA and 1~5%.
It is further preferred that the ingredient of the first layer coating includes 5~28% silicon oxynitride, 70~90% dioxy
SiClx and 2~5% silica solution, still more preferably, the ingredient of the first layer coating includes 10~25% silicon oxynitride,
72~85% silica and 2~5% silica solution；The ingredient of the second layer coating includes 30~50% nitrogen oxidation
Silicon, 20~35% silica, 20~35% silicon nitride, 2~5% silica solution and 2~5% PVA；The third layer
The ingredient of coating includes 10~25% silicon oxynitride, 65~85% silicon nitride, the PAA of 2~5% PVA and 2~5%.
The first layer coating with a thickness of 20~40 μm, the second layer coating with a thickness of 30~50 μm, described
Three-layer coating with a thickness of 50~100 μm.
Alcoholysis degree >=98% of the PVA；Molecular weight >=1250000 PAA.Product can be improved in the raw material of high quality
Quality, purity >=99% of the silicon oxynitride, the purity of the silica, silicon nitride and silica solution is >=99.99%.
Above-mentioned coating exempts to spray the application in crucible in preparation casting polysilicon.
A kind of casting polysilicon exempts to spray crucible, and above-mentioned coating is sprayed on the surface of silica crucible.
A kind of casting polysilicon exempts from the preparation method of spray crucible, successively sprays three layers of painting from inside to outside in quartz crucible surface
Layer.Its specific preparation process are as follows: first layer coating is sprayed in quartz crucible surface first, based on mass percentage, described the
The ingredient of one layer of coating includes 4.5~95% silicon oxynitride, 4.5~95% silica and 0.5~5% silica solution；
Then second layer coating is sprayed in first layer coating surface, based on mass percentage, the ingredient of the second layer coating includes 5
~50% silicon oxynitride, 0.5~50% silica, 0.5~50% silicon nitride, 0.5~5% silica solution and 0.5
~5% PVA；Finally third layer coating, based on mass percentage, the third layer coating are sprayed in second layer coating surface
Include 0.5~95% silicon oxynitride, 0.5~95% silicon nitride, the PAA of 0.5~5% PVA and 0.5~5%.
In above-mentioned method, the first layer coating with a thickness of 20~40 μm, the second layer coating with a thickness of
30~50 μm, the third layer coating with a thickness of 50~100 μm.
Above-mentioned method, alcoholysis degree >=98% of the PVA；Molecular weight >=1250000 PAA.
Nitrogen oxidation is utilized by preparing the coating of three layers of heterogeneity in high-purity silica pot inner wall in the preparation method
A kind of interphase as silicon nitride and silica of silicon, constitutive property not only and silicon nitride, but also have with silica relatively strong
Similitude, so itself and silicon nitride, silica have stronger binding force so that whole coating have bigger intensity and
Higher consistency reduces the quantity of impure point in silicon liquid, finally reduces ingot casting to be substantially reduced the risk that silicon nitride falls off
The quantity of red sector, improves the yield rate of ingot casting, and increases the photoelectric conversion efficiency of photovoltaic module.
Unless otherwise indicated, raw material according to the present invention can be obtained by being bought with market.
Compared with prior art, the present invention has the advantage that
Present invention utilizes silicon oxynitrides not only and silicon nitride, but also had stronger binding force with silica, solved earthenware
Crucible surface direct spraying silicon nitride, silicon nitride and the not strong problem of silica surface binding force.
By preparing the coating of three kinds of heterogeneities, the ingenious variation that three kinds of ingredients are utilized: first layer coating contains dioxy
SiClx and silicon oxynitride ingredient and sidewall of crucible have very strong binding force；Second layer coating contains silica, silicon oxynitride and nitrogen
SiClx belongs to the middle layer of first layer and third layer, first layer and third layer firm connection can be got up；Third layer nitrogen
Silicon and silicon oxynitride, it is both strong with second layer binding force, in turn ensure that silicon ingot smoothly demoulds, the sequence of three coatings also significant shadow
Ring the effect of coating.
In short, enhance the intensity and consistency of coating by the design of above-mentioned coating, reduce impurity in silicon ingot and
Defect improves the yield rate of silicon ingot, finally improves the stability and photoelectric conversion efficiency of photovoltaic module.
Specific embodiment
Below by specific embodiment, the invention will be further described, but protection scope of the present invention be not limited to it is following
Embodiment.
Embodiment 1
First layer coating is prepared, based on mass percentage, ingredient includes 10% silicon oxynitride, 85% titanium dioxide
Silicon, 5% silica solution, wherein the purity of purity >=99% of the silicon oxynitride, the silica and silica solution is both greater than
99.99%.
Second layer coating is prepared, based on mass percentage, ingredient includes 50% silicon oxynitride, 20% titanium dioxide
Silicon, 20% silicon nitride, 5% silica solution, 5% PVA, wherein purity >=99% of the silicon oxynitride, the titanium dioxide
The alcoholysis degree that the purity of silicon, silicon nitride and silica solution is both greater than 99.99%, PVA is 98%.
Third layer coating is prepared, based on mass percentage, ingredient includes 10% silicon oxynitride, 80% nitridation
Silicon, 5% PVA, 5% PAA, wherein the purity of purity >=99% of the silicon oxynitride, the silicon nitride is both greater than
The alcoholysis degree of 99.99%, PVA are that 98%, PAA molecular weight is 1250000.
Firstly, in quartz crucible surface even application first layer coating, then, in first layer coating surface even application
Two layers of coating, finally, in second layer coating surface even application third layer coating.The first layer coating layer thickness is 20~30 μ
M, the second layer coating layer thickness are 30~40 μm, and the third layer coating layer thickness is 80~100 μm.
Coating manufactured in the present embodiment is subjected to adhesive force test, as a result 845kPa, is much higher than common coating, i.e. stone
The adhesive force that English crucible surface directly sprays silicon nitride is 310kPa.The crucible for being coated with this coating is applied to casting polysilicon,
Then the polysilicon cast is sliced, obtains A piece (high-quality silicon wafer) yield and reach 92.8%, is obtained much higher than common coating
90.3% yield.This is because consistency (the 4.68g/cm of this coating3) and intensity be improved so that entering ingot casting
In impure point tail off, to ingot casting carry out Buddha's warrior attendant wire cutting when, accordingly due to impure point and chipping even collapse line probability become
It is few, so that whole slice yield is improved.In this way, greatly improving whole yield rate and production efficiency.
Embodiment 2
First layer coating is prepared, based on mass percentage, ingredient includes 20% silicon oxynitride, 76% titanium dioxide
Silicon, 4% silica solution, wherein the purity of purity >=99% of the silicon oxynitride, the silica and silica solution is both greater than
99.99%.
Second layer coating is prepared, based on mass percentage, ingredient includes 40% silicon oxynitride, 26% titanium dioxide
Silicon, 26% silicon nitride, 4% silica solution, 4% PVA, wherein purity >=99% of the silicon oxynitride, the titanium dioxide
The alcoholysis degree that the purity of silicon, silicon nitride and silica solution is both greater than 99.99%, PVA is 98%.
Third layer coating is prepared, based on mass percentage, ingredient includes 20% silicon oxynitride, 72% nitridation
Silicon, 4% PVA, 4% PAA, wherein the purity of purity >=99% of the silicon oxynitride, the silicon nitride is both greater than
The alcoholysis degree of 99.99%, PVA are that 98%, PAA molecular weight is 3000000.
Firstly, in quartz crucible surface even application first layer coating, then, in first layer coating surface even application
Two layers of coating, finally, in second layer coating surface even application third layer coating.The first layer coating layer thickness is 30~35 μ
M, second layer coating layer thickness are 40~45 μm, and third layer coating layer thickness is 65~80 μm.
Coating manufactured in the present embodiment is subjected to adhesive force test, as a result 903kPa, is much higher than common coating, i.e. stone
The adhesive force that English crucible surface directly sprays silicon nitride is 310kPa.The crucible for being coated with this coating is applied to casting polysilicon,
Then the polysilicon cast is sliced, obtains A piece (high-quality silicon wafer) yield and reach 93.2%, is obtained much higher than common coating
90.3% yield.This is because consistency (the 5.01g/cm of this coating3) and intensity be improved so that entering ingot casting
In impure point tail off, to ingot casting carry out Buddha's warrior attendant wire cutting when, accordingly due to impure point and chipping even collapse line probability become
It is few, so that whole slice yield is improved.In this way, greatly improving whole yield rate and production efficiency.
Embodiment 3
First layer coating is prepared, based on mass percentage, ingredient includes 25% silicon oxynitride, 72% titanium dioxide
Silicon, 3% silica solution, wherein the purity of purity >=99% of the silicon oxynitride, the silica and silica solution is both greater than
99.99%.
Second layer coating is prepared, based on mass percentage, ingredient includes 30% silicon oxynitride, 32% titanium dioxide
Silicon, 32% silicon nitride, 3% silica solution, 3% PVA, wherein purity >=99% of the silicon oxynitride, the titanium dioxide
The alcoholysis degree that the purity of silicon, silicon nitride and silica solution is both greater than 99.99%, PVA is 98%.
Third layer coating is prepared, based on mass percentage, ingredient includes 25% silicon oxynitride, 69% nitridation
Silicon, 3% PVA, 3% PAA, wherein the purity of purity >=99% of the silicon oxynitride, the silicon nitride is both greater than
The alcoholysis degree of 99.99%, PVA are that 98%, PAA molecular weight is 4000000.
Firstly, in quartz crucible surface even application first layer coating, then, in first layer coating surface even application
Two layers of coating, finally, in second layer coating surface even application third layer coating.The first layer coating layer thickness is 35~40 μ
M, second layer coating layer thickness are 45~50 μm, and third layer coating layer thickness is 50~65 μm.
Coating manufactured in the present embodiment is subjected to adhesive force test, as a result 914kPa, is much higher than common coating, i.e. stone
The adhesive force that English crucible surface directly sprays silicon nitride is 310kPa.The crucible for being coated with this coating is applied to casting polysilicon,
Then the polysilicon cast is sliced, obtains A piece (high-quality silicon wafer) yield and reach 93.8%, is obtained much higher than common coating
90.3% yield.This is because consistency (the 5.17g/cm of this coating3) and intensity be improved so that entering ingot casting
In impure point tail off, to ingot casting carry out Buddha's warrior attendant wire cutting when, accordingly due to impure point and chipping even collapse line probability become
It is few, so that whole slice yield is improved.In this way, greatly improving whole yield rate and production efficiency.
Comparative example 1
On the contrary, using technological parameter same as Example 3, but silicon oxynitride is not added, specific scheme is as follows:
First layer coating is prepared, based on mass percentage, 25% silicon nitride, 72% silica, 3% silicon is molten
Glue, wherein the purity of silicon nitride, silica and silica solution is both greater than 99.99%.
Second layer coating is prepared, based on mass percentage, 32% silica, 62% silicon nitride, 3% silicon is molten
Glue, 3% PVA, wherein the alcoholysis degree that the purity of silica, silicon nitride and silica solution is both greater than 99.99%, PVA is
98%.
Third layer coating is prepared, based on mass percentage, 94% silicon nitride, 3% PVA, 3% PAA, wherein
It is 4000000 that alcoholysis degree of the purity of silicon nitride greater than 99.99%, PVA, which is 98%, PAA molecular weight,.
Firstly, in quartz crucible surface even application first layer coating, then, in first layer coating surface even application
Two layers of coating, finally, in second layer coating surface even application third layer coating.The first layer coating layer thickness is 35~40 μ
M, second layer coating layer thickness are 45~50 μm, and third layer coating layer thickness is 50~65 μm.
Coating prepared by this comparative example carries out adhesive force test, as a result 356kPa, close to common coating, i.e., quartzy
The adhesive force that crucible surface directly sprays silicon nitride is 310kPa, but (strictly according to the facts far below the coating adhesion of addition silicon oxynitride
Apply example 1,2,3).Coating consistency is 3.11g/cm3, the crucible for being coated with this coating is applied to casting polysilicon, then will
The polysilicon cast is sliced, and is obtained A piece (high-quality silicon wafer) yield and is reached 90.8%, 90.3% obtained higher than common coating
Yield.I.e. yield is slightly above common coating, but far below the coating of addition silicon oxynitride.
Comparative example 2
First layer coating is prepared, based on mass percentage, ingredient includes 30% silicon oxynitride, 32% titanium dioxide
Silicon, 32% silicon nitride, 3% silica solution, 3% PVA, wherein purity >=99% of the silicon oxynitride, the titanium dioxide
The alcoholysis degree that the purity of silicon, silicon nitride and silica solution is both greater than 99.99%, PVA is 98%.
Second layer coating is prepared, based on mass percentage, ingredient includes 25% silicon oxynitride, 72% titanium dioxide
Silicon, 3% silica solution, wherein the purity of purity >=99% of the silicon oxynitride, the silica and silica solution is both greater than
99.99%.
Third layer coating is prepared, based on mass percentage, ingredient includes 25% silicon oxynitride, 69% nitridation
Silicon, 3% PVA, 3% PAA, wherein the purity of purity >=99% of the silicon oxynitride, the silicon nitride is both greater than
The alcoholysis degree of 99.99%, PVA are that 98%, PAA molecular weight is 4000000.
Firstly, in quartz crucible surface even application first layer coating, then, in first layer coating surface even application
Two layers of coating, finally, in second layer coating surface even application third layer coating.The first layer coating layer thickness is 35~40 μ
M, second layer coating layer thickness are 45~50 μm, and third layer coating layer thickness is 50~65 μm.
Coating prepared by this comparative example carries out adhesive force test, as a result 611kPa, is significantly higher than common coating, i.e.,
The adhesive force that quartz crucible surface directly sprays silicon nitride is 310kPa.But far below the coating adhesion of addition silicon oxynitride
(such as embodiment 1,2,3).Coating consistency is 4.25g/cm3, the crucible for being coated with this coating is applied to casting polysilicon, so
The polysilicon cast is sliced afterwards, A piece (high-quality silicon wafer) yield is obtained and reaches 91.6%, obtained higher than common coating
90.3% yield, but it is far below the coating of embodiment 1,2,3.
Claims (9)
1. a kind of casting polysilicon exempts to spray crucible coating layer, which is characterized in that the coating successively includes three-layer coating from inside to outside,
In based on mass percentage,
The ingredient of first layer coating include 4.5 ~ 95% silicon oxynitride, 4.5 ~ 95% silica and 0.5 ~ 5% silica solution；
The ingredient of second layer coating include 5 ~ 50% silicon oxynitride, 0.5 ~ 50% silica, 0.5 ~ 50% silicon nitride, 0.5
~ 5% silica solution and 0.5 ~ 5% PVA；
The ingredient of third layer coating includes 0.5 ~ 95% silicon oxynitride, 0.5 ~ 95% silicon nitride, 0.5 ~ 5% PVA and 0.5 ~ 5%
PAA.
2. casting polysilicon according to claim 1 exempts to spray crucible coating layer, which is characterized in that based on mass percentage,
The ingredient of the first layer coating include 5 ~ 70% silicon oxynitride, 25 ~ 90% silica and 1 ~ 5% silica solution；
The ingredient of the second layer coating include 10 ~ 50% silicon oxynitride, 5 ~ 40% silica, 5 ~ 40% silicon nitride, 1 ~
5% silica solution and 1 ~ 5% PVA；
The ingredient of the third layer coating include 10 ~ 35% silicon oxynitride, 60 ~ 85% silicon nitride, 1 ~ 5% PVA's and 1 ~ 5%
PAA。
3. casting polysilicon according to claim 1 or 2 exempts to spray crucible coating layer, which is characterized in that the first layer coating
With a thickness of 20 ~ 40 μm, the second layer coating with a thickness of 30 ~ 50 μm, the third layer coating with a thickness of 50 ~ 100 μm.
4. casting polysilicon according to claim 1 or 2 exempts to spray crucible coating layer, which is characterized in that the alcoholysis degree of the PVA
≥98%；Molecular weight >=1250000 PAA.
5. any coating exempts to spray the application in crucible in preparation casting polysilicon in claim 1 ~ 4.
6. a kind of casting polysilicon exempts to spray crucible, which is characterized in that any in the surface of silica crucible spraying claim 1 ~ 4
The coating.
7. a kind of casting polysilicon exempts to spray the preparation method of crucible, it is characterised in that: quartz crucible surface from inside to outside successively
Spray three-layer coating；
First quartz crucible surface spray first layer coating, based on mass percentage, the first layer coating at subpackage
Include 4.5 ~ 95% silicon oxynitride, 4.5 ~ 95% silica and 0.5 ~ 5% silica solution；
Then second layer coating, based on mass percentage, the ingredient of the second layer coating are sprayed in first layer coating surface
Including 5 ~ 50% silicon oxynitride, 0.5 ~ 50% silica, 0.5 ~ 50% silicon nitride, 0.5 ~ 5% silica solution and 0.5 ~ 5%
PVA；
Third layer coating finally is sprayed in second layer coating surface, based on mass percentage, the third layer coating includes
0.5 ~ 95% silicon oxynitride, 0.5 ~ 95% silicon nitride, the PAA of 0.5 ~ 5% PVA and 0.5 ~ 5%.
8. according to the method described in claim 7, it is characterized by: the first layer coating with a thickness of 20 ~ 40 μm, described
Two layers of coating with a thickness of 30 ~ 50 μm, the third layer coating with a thickness of 50 ~ 100 μm.
9. according to the method described in claim 7, it is characterized by: alcoholysis degree >=98% of the PVA；The PAA molecular weight >=
1250000。
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711354112.7A CN108046846B (en) | 2017-12-15 | 2017-12-15 | A kind of casting polysilicon exempts to spray crucible coating layer and preparation method thereof |
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