CN108046846A - 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 cast polysilicon exempt from spray crucible coating layer and preparation method thereof, the coating includes three layer coating successively 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% Ludox;The ingredient of second layer coating includes 5~50% silicon oxynitride, 0.5~50% silica, 0.5~50% silicon nitride, 0.5~5% Ludox 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.Present invention utilizes silicon oxynitride both and silicon nitride, the characteristics of again and silicon oxynitride combination power is strong, pass through rational composition design, solve the problems, such as that silicon nitride and sidewall of crucible combination power is 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, improve 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 technology
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.Higher photoelectric conversion efficiency in order to obtain, impurity and the defect for casting polysilicon are more few better.Polysilicon is being cast
In the process, generally use high-purity silica crucible as container, but silicon material is in the case of 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 outflow of high temperature, it is possible to cause serious security incident.Cause
This, to solve the problems, such as this, 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 is smoothed out simultaneously smoothly demoulding.But although by silicon nitride spray finishing
In crucible as releasing 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 is not strong with silica crucible combination power in itself so that silicon nitride is easily fallen 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 when follow-up Buddha's warrior attendant wire cutting and breaks, causes production accident.3rd, nitrogen
SiClx is in itself 45 °~50 ° with the angle of wetting of silicon liquid, and in the case where angle of wetting is less than 90 °, solid liquid interface still has wetting
Situation, so not only so that silicon nitride in nitrogen diffuse more readily into inside silicon liquid the pollution caused to silicon ingot, but also
Demoulding possibility that is not smooth or even splitting ingot is added, 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 the glass structure layer containing Ludox~gel, so add the stop to impurity, but still without solving silicon nitride and two
The problem of silica combination power is not strong, the silicon nitride on surface still have the risk polluted in the silicon liquid fallen into.
The Chinese specialty of Application No. 201620841199.5 discloses a kind of barium silicate crystal layer 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 that impurity is expanded by bubble to silicon ingot inside crucible
It dissipates, reduces pollution of the crucible to silicon ingot.But silicic acid crystal of barium contains barium metal in itself, 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 employ the incorporation 3.8wt% nano silicon dioxides 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.), so as to add silicon nitride into
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 of high cost, it is not easy to prepare, and is 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.
The content of the invention
Object of the present invention is to provide a kind of casting polysilicons to exempt to spray crucible coating layer and its application.
Another object of the present invention is to provide a kind of casting polysilicon to exempt to spray crucible.
Another object of the present invention is to provide a kind of preparation method for casting polysilicon and exempting from spray crucible.
Technical scheme is specially:
A kind of casting polysilicon exempts to spray crucible coating layer, which includes three layer coating successively from inside to outside, wherein by quality
Percentage composition meter,
The ingredient of first layer coating includes 4.5~95% silicon oxynitride, 4.5~95% silica and 0.5~5%
Ludox, 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% Ludox 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% Ludox;The ingredient of the second layer coating includes 10~50% silicon oxynitride, 5~
40% silica, 5~40% silicon nitride, 1~5% Ludox and 1~5% PVA;The third layer coating into
Point include 10~35% silicon oxynitride, 60~85% silicon nitride, 1~5% PVA and 1~5% PAA.
It is further preferred that the ingredient of the first layer coating includes 5~28% silicon oxynitride, 70~90% dioxy
SiClx and 2~5% Ludox, still more preferably, the ingredient of the first layer coating include 10~25% silicon oxynitride,
72~85% silica and 2~5% Ludox;The ingredient of the second layer coating includes 30~50% nitrogen oxidation
Silicon, 20~35% silica, 20~35% silicon nitride, 2~5% Ludox and 2~5% PVA;The third layer
The ingredient of coating includes 10~25% silicon oxynitride, 65~85% silicon nitride, 2~5% PVA and 2~5% PAA.
The thickness of the first layer coating is 20~40 μm, and the thickness of the second layer coating is 30~50 μm, described the
The thickness of three layer coating is 50~100 μm.
Alcoholysis degree >=98% of the PVA;PAA molecular weight >=1250000.The raw material of high quality can improve product
Quality, purity >=99% of the silicon oxynitride, the purity of the silica, silicon nitride and Ludox is >=99.99%.
Application of the above-mentioned coating in preparing casting polysilicon and exempting to spray crucible.
A kind of casting polysilicon exempts to spray crucible, in the above-mentioned coating of the surface spraying of silica crucible.
A kind of polysilicon that casts exempts to spray the preparation method of crucible, and three layers of painting are sprayed successively from inside to outside in quartz crucible surface
Layer.Its specific preparation process is: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% Ludox;
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% Ludox and 0.5
~5% PVA;Finally third layer coating, based on mass percentage, the third layer coating are sprayed in second layer coating surface
The silicon oxynitride for including 0.5~95%, 0.5~95% silicon nitride, 0.5~5% PVA and 0.5~5% PAA.
In above-mentioned method, the thickness of the first layer coating is 20~40 μm, and the thickness of the second layer coating is
30~50 μm, the thickness of the third layer coating is 50~100 μm.
Above-mentioned method, alcoholysis degree >=98% of the PVA;PAA molecular weight >=1250000.
The preparation method by preparing the coating of three layers of heterogeneity in high-purity silica pot inner wall, make use of nitrogen oxidation
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 it is stronger with reference to power so that whole coating have bigger intensity and
Higher consistency so as to be substantially reduced the risk that silicon nitride comes off, reduces the quantity of impure point in silicon liquid, finally reduces ingot casting
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 invention has the advantages that:
Present invention utilizes silicon oxynitride not only and silicon nitride, but also with silica there is stronger combination power, solves earthenware
The problem of crucible surface direct spraying silicon nitride, silicon nitride and not strong silica surface combination power.
By preparing the coating of three kinds of heterogeneities, the ingenious variation that make use of three kinds of ingredients:First layer coating contains dioxy
SiClx and silicon oxynitride ingredient and sidewall of crucible have very strong combination power;Second layer coating contains silica, silicon oxynitride and nitrogen
SiClx belongs to the interlayer of first layer and third layer, and first layer and third layer firm connection can get up;Third layer nitrogen
Silicon and silicon oxynitride, it is both strong with second layer combination power, in turn ensure that silicon ingot smoothly demoulds, the orders of three coatings also notable shadow
Ring the effect of coating.
In short, by the design of above-mentioned coating, enhance the intensity and consistency of 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% Ludox, wherein, purity >=99% of the silicon oxynitride, the purity of the silica and Ludox 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% Ludox, 5% PVA, wherein, purity >=99% of the silicon oxynitride, the titanium dioxide
The alcoholysis degree that the purity of silicon, silicon nitride and Ludox 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, purity >=99% of the silicon oxynitride, the purity of the silicon nitride is both greater than
The alcoholysis degree of 99.99%, PVA are that 98%, PAA molecular weight is 1250000.
First, 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, far above 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 cut into slices, obtains A pieces (high-quality silicon chip) yield and reach 92.8%, obtained far above common coating
90.3% yield.This is because consistency (the 4.68g/cm of this coating3) and intensity be improved so that enter 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 section yield is improved.In this way, greatly improve 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% Ludox, wherein, purity >=99% of the silicon oxynitride, the purity of the silica and Ludox 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% Ludox, 4% PVA, wherein, purity >=99% of the silicon oxynitride, the titanium dioxide
The alcoholysis degree that the purity of silicon, silicon nitride and Ludox 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, purity >=99% of the silicon oxynitride, the purity of the silicon nitride is both greater than
The alcoholysis degree of 99.99%, PVA are that 98%, PAA molecular weight is 3000000.
First, 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, far above 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 cut into slices, obtains A pieces (high-quality silicon chip) yield and reach 93.2%, obtained far above common coating
90.3% yield.This is because consistency (the 5.01g/cm of this coating3) and intensity be improved so that enter 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 section yield is improved.In this way, greatly improve 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% Ludox, wherein, purity >=99% of the silicon oxynitride, the purity of the silica and Ludox 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% Ludox, 3% PVA, wherein, purity >=99% of the silicon oxynitride, the titanium dioxide
The alcoholysis degree that the purity of silicon, silicon nitride and Ludox 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, purity >=99% of the silicon oxynitride, the purity of the silicon nitride is both greater than
The alcoholysis degree of 99.99%, PVA are that 98%, PAA molecular weight is 4000000.
First, 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, far above 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 cut into slices, obtains A pieces (high-quality silicon chip) yield and reach 93.8%, obtained far above common coating
90.3% yield.This is because consistency (the 5.17g/cm of this coating3) and intensity be improved so that enter 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 section yield is improved.In this way, greatly improve 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 Ludox 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 Ludox 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,
Alcoholysis degree of the purity of silicon nitride more than 99.99%, PVA is that 98%, PAA molecular weight is 4000000.
First, 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
Crucible surface directly sprays the adhesive force of silicon nitride for 310kPa, but is far below the coating adhesion of addition silicon oxynitride (strictly according to the facts
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 cut into slices, and is obtained A pieces (high-quality silicon chip) 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% Ludox, 3% PVA, wherein, purity >=99% of the silicon oxynitride, the titanium dioxide
The alcoholysis degree that the purity of silicon, silicon nitride and Ludox 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% Ludox, wherein, purity >=99% of the silicon oxynitride, the purity of the silica and Ludox 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, purity >=99% of the silicon oxynitride, the purity of the silicon nitride is both greater than
The alcoholysis degree of 99.99%, PVA are that 98%, PAA molecular weight is 4000000.
First, 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 cut into slices afterwards, A pieces (high-quality silicon chip) yield is obtained and reaches 91.6%, obtained higher than common coating
90.3% yield, but far below the coating of embodiment 1,2,3.
Claims (10)
1. a kind of casting polysilicon exempts to spray crucible coating layer, which is characterized in that the coating includes three layer coating successively from inside to outside,
In based on mass percentage,
The ingredient of first layer coating includes 4.5~95% silicon oxynitride, 4.5~95% silica and 0.5~5% silicon
Colloidal sol;
The ingredient of second layer coating includes 5~50% silicon oxynitride, 0.5~50% silica, 0.5~50% nitridation
Silicon, 0.5~5% Ludox 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. it is according to claim 1 casting polysilicon exempt from spray crucible coating layer, which is characterized in that the first layer coating into
Point include 5~70% silicon oxynitride, 25~90% silica and 1~5% Ludox;
The ingredient of the second layer coating includes 10~50% silicon oxynitride, 5~40% silica, 5~40% nitrogen
SiClx, 1~5% Ludox and 1~5% PVA;
The ingredient of the third layer coating includes 10~35% silicon oxynitride, 60~85% silicon nitride, 1~5% PVA 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
Thickness for 20~40 μm, the thickness of the second layer coating is 30~50 μm, and the thickness of the third layer coating is 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%;PAA molecular weight >=1250000.
5. application of any coating in preparing casting polysilicon and exempting to spray crucible in Claims 1 to 4.
6. a kind of casting polysilicon exempts to spray crucible, which is characterized in that appoints in the surface spraying Claims 1 to 4 of silica crucible
Coating described in one.
7. a kind of polysilicon that casts exempts to spray the preparation method of crucible, it is characterised in that:In quartz crucible surface from inside to outside successively
Spray three layer coating.
8. according to the method described in claim 7, it is characterized in that:First layer coating is sprayed in quartz crucible surface first, is pressed
Mass percentage meter, the ingredient of the first layer coating include 4.5~95% silicon oxynitride, 4.5~95% titanium dioxide
Silicon and 0.5~5% Ludox;
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% Ludox
With 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, 0.5~5% PVA and 0.5~5% PAA.
9. the method according to claim 7 or 8, it is characterised in that:The thickness of the first layer coating is 20~40 μm, institute
The thickness of second layer coating is stated as 30~50 μm, the thickness of the third layer coating is 50~100 μm.
10. according to the method described in claim 7, it is characterized in that:Alcoholysis degree >=98% of the PVA;The PAA molecular weight
≥1250000。
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Cited By (2)
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CN111589678A (en) * | 2020-05-29 | 2020-08-28 | 徐州协鑫太阳能材料有限公司 | Preparation method of compact quartz crucible high-purity coating |
CN112536200A (en) * | 2019-09-21 | 2021-03-23 | 中材江苏太阳能新材料有限公司 | Side wall improved coating crucible for ingot single polycrystal and preparation method thereof |
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CN101942693A (en) * | 2009-07-08 | 2011-01-12 | 合晶科技股份有限公司 | Quartz glass crucible with protective layer and manufacturing method thereof |
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CN112536200A (en) * | 2019-09-21 | 2021-03-23 | 中材江苏太阳能新材料有限公司 | Side wall improved coating crucible for ingot single polycrystal and preparation method thereof |
CN112536200B (en) * | 2019-09-21 | 2022-04-01 | 中材江苏太阳能新材料有限公司 | Side wall improved coating crucible for ingot single polycrystal and preparation method thereof |
CN111589678A (en) * | 2020-05-29 | 2020-08-28 | 徐州协鑫太阳能材料有限公司 | Preparation method of compact quartz crucible high-purity coating |
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