CN101942693A - Quartz glass crucible with protective layer and manufacturing method thereof - Google Patents
Quartz glass crucible with protective layer and manufacturing method thereof Download PDFInfo
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- CN101942693A CN101942693A CN2009101583779A CN200910158377A CN101942693A CN 101942693 A CN101942693 A CN 101942693A CN 2009101583779 A CN2009101583779 A CN 2009101583779A CN 200910158377 A CN200910158377 A CN 200910158377A CN 101942693 A CN101942693 A CN 101942693A
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- silicon oxynitride
- mixolimnion
- silicon
- quartz glass
- glass crucibles
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Abstract
The invention discloses a manufacturing method of a quartz glass crucible with a protective layer. The method comprises the following steps: providing a quartz glass crucible main body; forming at least one first silicon oxynitride layer on the inside of the quartz glass crucible main body; then forming at least one second silicon oxynitride layer on the first silicon oxynitride layer; and finally forming a silicon nitride layer on the second silicon oxynitride layer, wherein the first silicon oxynitride layer and the second silicon oxynitride layer are both formed by SiO2 and Si3N4 or the silicon oxynitride material; the Si3N4 content in the second silicon oxynitride layer is higher than that in the first silicon oxynitride layer, and the silicon nitride layer is formed by Si3N4. By using the method of the invention, the oxygen atoms can be prevented from penetrating in silicate melt; by adjusting the content of Si3N4 and/or the content of SiO2, the thickness of each layered structure can be controlled; and the service life of the quartz glass crucible can be prolonged.
Description
Technical field
The present invention relates to a kind of manufacture method with quartz glass crucibles of protective layer, especially a kind of silicon nitride concentration that increases gradually in the quartz glass crucibles inboard is to form the method that can stablize the silicon oxynitride protective layer that is attached to quartz glass crucibles.
Background technology
Please referring to shown in Figure 2, the crucible 30 that generally is used for the long brilliant usefulness of semi-conductor silicon wafer normally will have highly purified silicon and be melted in the quartz glass crucibles and form the molten soup 40 of silicon, again crystal seed is inserted in the molten soup of silicon, and with suitable speed rotation crystal seed and gradually with its drawing and form the silicon crystal bar 50 that meets size up, this kind method is called " monocrystalline vertical pulling method (Czochralski; CZ method) ", the Silicon Wafer that silicon crystal bar 50 cut into slices afterwards again, grind, processing procedure such as polishing can obtain required specification.
And the crucible 30 that is used for the long brilliant usefulness of semi-conductor silicon wafer is generally the material of silica glass (being silicon-dioxide); Yet, owing to contain Sauerstoffatom in the silica glass material, so when being loaded with the molten soup 40 of pyritous silicon in the quartz glass crucibles 30, Sauerstoffatom can be fused into silicon from the internal surface diffusion back of quartz glass crucibles 30 and melt the soup 40, and pollute the molten soup 40 of silicon, and its purity is descended.Wherein, oxygen concn relation with other parameter in vertical pulling method monocrystalline making processes is as follows:
[O]
Si＝A
Rvk
eC
m＝A
cD(C
c-C
m)/δ
c-A
mD(C
a-C
m)/δ
m
Wherein [O]
SiRepresent the oxygen level of the molten soup of silicon, A
RBe crystal bar sectional area, A
CBe the area at quartz glass crucibles and the molten soup interface of silicon, A
mBe the area at molten soup of silicon and peripheral atmosphere interface, v is a pulling rate, k
eBe the balance segregation coefficient of oxygen, C
mBe oxygen concentration in molten soup, C
CBe the concentration of oxygen on the quartz crucible surface, C
aBe the concentration of oxygen in peripheral atmosphere, δ
cBe the diffusion boundary layer thickness of quartz crucible and the molten soup of silicon, δ
mDiffusion boundary layer thickness for molten soup of silicon and peripheral atmosphere.
Therefore, if will reduce the concentration of oxygen in the molten soup of silicon, then can take following several method:
1. at the inboard protective layer that forms of crucible;
2. the size that increases quartz glass crucibles is to reduce A
C/ A
mRatio;
3. reduce crucible rotation or add magnetic field, to reduce C
CAnd increase δ
c
4. improve the flow velocity of argon gas or reduce processing pressure to increase the rate of volatilization of oxygen silicide (SiO species).
And the method for the most normal use at present is to reduce crucible rotation or add magnetic field effect at long brilliant processing procedure to reduce the concentration of oxygen at the quartz glass crucibles internal surface, avoids Sauerstoffatom to fuse into to silicon in the molten soup through high temperature from quartz glass crucibles.
Existing method, No. 0753605 patent of No. 20020086119 patent or Europe disclosed as the U.S., it is to form metal oxide (as barium oxide), oxyhydroxide, carbide or silicide etc. in the inboard of quartz glass crucibles, yet, if formed protective layer is an oxide compound, then the purpose of this protective layer is in the life-span that increases quartz glass crucibles, and is less for the influence of oxygen level; In addition, no matter use materials such as oxide compound, oxyhydroxide, all can produce between protective layer and the quartz glass crucibles closely bonded problem.
And for example the U.S. the 4th, 741, and No. 925 the patent case discloses a kind of method, and it is with ammonia (NH
3) and silicon tetrachloride (SiCl
4) gas reaction and at the inboard coating that forms of quartz glass crucibles, then rotate this quartz glass crucibles so that this coating is even, be heated at last and form protective layer, and the thickness of protective layer is about 2～5 Mills (mil).Yet utilize the uncontrollable desired thickness of existing method, and because of the problem of material, and cause between silicon nitride and the quartz glass crucibles closely bonded problem equally easily.
Summary of the invention
The inventor can't obtain to adhere to protective layer good and the energy control thickness with quartz glass crucibles in view of existing method; therefore through after long research and the continuous test, invent out the manufacture method that this has the quartz glass crucibles of protective layer finally.
The object of the present invention is to provide a kind of silicon nitride concentration that increases gradually in the quartz glass crucibles inboard to form the method that to stablize the silicon oxynitride protective layer that is attached to quartz glass crucibles.
For reaching above-mentioned purpose, the present invention has the manufacture method of the quartz glass crucibles of protective layer, and it comprises:
One quartz glass crucibles body is provided;
Form at least one first silicon oxynitride mixolimnion in the inboard of this quartz glass crucibles body;
On this first silicon oxynitride mixolimnion, form at least one second silicon oxynitride mixolimnion again;
Form a silicon nitride layer in this second silicon oxynitride mixolimnion again, this first silicon oxynitride mixolimnion and the second silicon oxynitride mixolimnion are all by silicon-dioxide (SiO
2) and silicon nitride (Si
3N
4) form, wherein the silicon nitride of this second silicon oxynitride mixolimnion ratio that accounts for the second silicon oxynitride mixolimnion is many than the ratio that the silicon nitride of the first silicon oxynitride mixolimnion accounts for the first silicon oxynitride mixolimnion, this silicon nitride layer is made up of silicon nitride.
Wherein, the dioxide-containing silica of this first silicon oxynitride mixolimnion is less than the 100wt% of the whole first silicon oxynitride mixolimnion, and more than or equal to 50wt%, and the content of silicon nitride is the 0wt% greater than the whole first silicon oxynitride mixolimnion, and is less than or equal to 50wt%; The dioxide-containing silica of this second silicon oxynitride mixolimnion is less than the 50wt% of the whole first silicon oxynitride mixolimnion, and greater than 0wt%, and the content of silicon nitride is the 50wt% greater than the whole first silicon oxynitride mixolimnion, and less than 100wt%.
Preferably, form this at least one first silicon oxynitride mixolimnion, this at least one second silicon oxynitride mixolimnion and this silicon nitride layer in the inboard of this quartz glass crucibles body in the agglomerating mode.
Preferably, the silicon oxynitride mixolimnion of quartz glass crucibles internal layer and the agglomerating pressure of silicon nitride layer are 20～100 handkerchiefs (Pa), and the agglomerating temperature is 1800～2000 ℃.
Preferably, the material of this silicon-dioxide and silicon nitride is all the particle of 5～500 μ m.
The present invention is still about a kind of quartz glass crucibles with protective layer, and it is made with above-mentioned manufacture method.
About a kind of quartz glass crucibles with protective layer, it comprises again in the present invention:
One quartz glass crucibles body; And
One silicon oxynitride (silicon oxynitride) protective layer, it is formed on this quartz glass crucibles body inboard, and this silicon oxynitride protective layer has cumulative silicon nitride and silicon-dioxide (Si from a side that contacts this quartz glass crucibles body towards other side
3N
4/ SiO
2) ratio;
One silicon nitride layer, it is arranged at the in addition side of this silicon oxynitride protective layer noncontact in this quartz glass crucibles body.
Preferably, this silicon oxynitride protective layer comprises at least one first silicon oxynitride mixolimnion of the inboard that is formed on this quartz glass crucibles body, at least one second silicon oxynitride mixolimnion on surface that is formed on this first silicon oxynitride mixolimnion and a silicon nitride layer that is formed at the surface of this second silicon oxynitride mixolimnion; Wherein the dioxide-containing silica of this first silicon oxynitride mixolimnion is less than the 100wt% of the whole first silicon oxynitride mixolimnion, and more than or equal to 50wt%, and the content of silicon nitride is the 0wt% greater than the whole first silicon oxynitride mixolimnion, and is less than or equal to 50wt%; The dioxide-containing silica of this second silicon oxynitride mixolimnion is less than the 50wt% of the whole second silicon oxynitride mixolimnion, and greater than 0wt%, and the content of silicon nitride is the 50wt% greater than the whole second silicon oxynitride mixolimnion, and less than 100wt%.
Best is, this silicon oxynitride protective layer is formed at least one first silicon oxynitride mixolimnion of inboard of this quartz glass crucibles body by this and at least one second silicon oxynitride mixolimnion on this surface that is formed on this first silicon oxynitride mixolimnion is formed.
Preferably, the material of this silicon-dioxide and silicon nitride is all the particle of grain size 5～500 μ m.
Because the present invention reduces silica composition gradually in the inboard of quartz glass crucibles body; and relatively increase the silicon nitride composition; so in the not directly combination and the irrelevant fully silicon nitride material of silicon-dioxide of the inboard of quartz glass crucibles body; therefore silicon nitride layer of the present invention can and have good tack by the silicon oxynitride protective layer between this quartz glass crucibles body, so can increase the life-span of this quartz glass crucibles.Moreover the present invention can adjust the thickness of the first silicon oxynitride mixolimnion, the second silicon oxynitride mixolimnion and nitride layer according to desired thickness, so the present invention controls the thickness of silicon oxynitride protective layer easily.
Description of drawings
Figure 1A to Fig. 1 D is the schematic flow sheet of making method of the present invention.
Fig. 2 is the user mode side sectional view of existing quartz glass crucibles.
[primary clustering nomenclature]
10 quartz glass crucibles bodies, 20 silicon oxynitride protective layers
21 first silicon oxynitride mixolimnions, 22 second silicon oxynitride mixolimnions
23 silicon nitride layers, 30 crucibles
40 silicon melt soup 50 silicon crystal bars
Embodiment
Please referring to shown in Figure 1, the present invention has the manufacture method of the quartz glass crucibles of protective layer, and it comprises: a quartz glass crucibles body 10 (Figure 1A) is provided; Pressure sintering in the inboard of this quartz glass crucibles body 10 with 20～100 handkerchiefs forms at least one first silicon oxynitride mixolimnion 21 (Figure 1B), pressure sintering with 20～100 handkerchiefs forms at least one second silicon oxynitride mixolimnion 22 (Fig. 1 C) on this first silicon oxynitride mixolimnion 21 again, form a silicon nitride layer 23 (Fig. 1 D) in these second silicon oxynitride mixolimnion, 22 pressure sinterings with 20～100 handkerchiefs again, this first silicon oxynitride mixolimnion 21 and the second silicon oxynitride mixolimnion 22 are all by silicon-dioxide (SiO
2) and silicon nitride (Si
3N
4) form, this silicon nitride layer 23 is made up of silicon nitride;
Wherein the dioxide-containing silica of this first silicon oxynitride mixolimnion 21 is less than the 100wt% of the whole first silicon oxynitride mixolimnion, and more than or equal to 50wt%, and silicon nitride content is the 0wt% greater than the whole first silicon oxynitride mixolimnion, and is less than or equal to 50wt%;
Wherein the dioxide-containing silica of this second silicon oxynitride mixolimnion 22 is less than the 50wt% of whole first silicon oxynitride layer, and greater than 0wt%, and the content of silicon nitride is the 50wt% greater than the whole first silicon oxynitride mixolimnion, and less than 100wt%;
Wherein employed silicon-dioxide and silicon nitride material are all the particle of 5～500 μ m.
Because the manufacture method of quartz glass crucibles body can be known for the person with usual knowledge in their respective areas, all discloses the manufacture method of quartz glass crucibles body as the 6th, 853, No. 673 patents of the 4th, 416, No. 680 patents of the U.S. and the U.S..
Therefore; please referring to Fig. 1 D; quartz glass crucibles with protective layer of the present invention; it comprises a quartz glass crucibles body 10, is formed on a silicon oxynitride protective layer 20 and a silicon nitride layer 23 of these quartz glass crucibles body 10 inboards, and this silicon oxynitride protective layer 20 has cumulative silicon nitride and silicon-dioxide (Si from a side that contacts this quartz glass crucibles body 10 towards other side
3N
4/ SiO
2) ratio, this silicon oxynitride protective layer 20 comprises by at least one first silicon oxynitride mixolimnion 21 and at least one second silicon oxynitride mixolimnion 22 of being formed on the surface of this first silicon oxynitride mixolimnion 21, this silicon nitride layer 23 is formed on the surface of this second silicon oxynitride mixolimnion 22, is the silicon nitride layer 23 of pure silicon nitride material to make this silicon oxynitride protective layer 20 in the side in addition of this quartz glass crucibles body 10 of contact; Wherein the dioxide-containing silica of this first silicon oxynitride mixolimnion 21 is less than the 100wt% of the whole first silicon oxynitride mixolimnion 21, and more than or equal to 50wt%, and the content of silicon nitride is the 0wt% greater than the whole first silicon oxynitride mixolimnion, and is less than or equal to 50wt%; The dioxide-containing silica of this second silicon oxynitride mixolimnion 22 is less than the 50wt% of the whole second silicon oxynitride mixolimnion 22, and greater than 0wt%, and the content of silicon nitride is the 50wt% greater than the whole first silicon oxynitride mixolimnion, and less than 100wt%.
Embodiment
Example 1
Heat and the fused silica material by in 2000 ℃ temperature, starching reactor, and form the quartz glass crucibles body with the electric arc electricity; Again with ratio uniform mixing SiO 2 powder (powder diameter size 75～300 μ m) and the alpha-silicon nitride powders (powder diameter size 5～200 μ m) of 75wt% and 25wt%, the mixed powder gross weight is 50 g, mode with the rotary integral quartz glass crucibles after inserting makes blended powder material be evenly distributed on the inboard of this quartz glass crucibles body, keeps the W-response environment and sinters it into one first silicon oxynitride mixolimnion in the pressure of 50 handkerchiefs and 1900 ℃ temperature; After electric arc electricity slurry reactor shifts out crucible, after treating that the quartz glass crucibles temperature descends, again with ratio uniform mixing SiO 2 powder (powder diameter size 75～300 μ m) and the alpha-silicon nitride powders (powder diameter size 5～200 μ m) of 50wt% and 50wt%, the mixed powder gross weight is 50 g, mode with the rotary integral quartz glass crucibles after inserting makes blended powder material be evenly distributed on this first silicon oxynitride mixolimnion surface, keeps the W-response environment and sinters it into another first silicon oxynitride mixolimnion in the pressure of 50 handkerchiefs and 1900 ℃ temperature; After electric arc electricity slurry reactor shifts out crucible, after treating that the silica glass temperature descends, again with ratio uniform mixing SiO 2 powder and alpha-silicon nitride powders mixed silica powder (powder diameter size 75～300 μ m) and the alpha-silicon nitride powders (powder diameter size 5～200 μ m) of 25wt% and 75wt%, the mixed powder gross weight is 50 g, insert the back and make blended powder material be evenly distributed on this another first silicon oxynitride mixolimnion surface, keep the W-response environment and sinter it into second silicon oxynitride mixolimnion in the pressure of 50 handkerchiefs and 1900 ℃ temperature in the mode of rotary integral quartz glass crucibles; After electric arc electricity slurry reactor shifts out crucible, after treating that the silica glass temperature descends, again the alpha-silicon nitride powders of 100wt% is inserted on this second silicon oxynitride mixolimnion surface, the powder gross weight is 50 g, sinters it into silicon nitride layer in the mode of rotary integral quartz glass crucibles and with the pressure of 50 handkerchiefs and 1900 ℃ temperature.The total thickness of the first silicon oxynitride mixolimnion of finishing, the second silicon oxynitride mixolimnion and silicon nitride layer etc. is about 10 μ m.
Therefore the silicon oxynitride protective layer of present embodiment is made up of two layers the first silicon oxynitride mixolimnion and one deck second silicon oxynitride mixolimnion.
Example 2
Heat and the fused silica material by in 2000 ℃ temperature, starching reactor, and form the quartz glass crucibles body with the electric arc electricity; Again with ratio uniform mixing SiO 2 powder and the alpha-silicon nitride powders of 90wt% and 10wt%, the mixed powder gross weight is 50 g, again the mode of its rotary integral quartz glass crucibles is made powder be evenly distributed on the inboard of this quartz glass crucibles body, and sinter it into one first silicon oxynitride mixolimnion with the pressure of the temperature of 50 handkerchiefs and 1900 ℃; After electric arc electricity slurry reactor shifts out crucible, after treating that the quartz glass crucibles temperature descends, again SiO 2 powder and alpha-silicon nitride powders are repeated above-mentioned steps with the ratio (gross weight is all 50 g) of 80wt% and 20wt%, 70wt% and 30wt%, 60wt% and 40wt% and 50wt% and 50wt% and in regular turn the mode of rotary integral quartz glass crucibles make powder be uniformly distributed in the inboard and sintering of crucible and storehouse forms five first silicon oxynitride mixolimnions; After electric arc electricity slurry reactor shifts out crucible, after treating that the quartz glass crucibles temperature descends, again with ratio uniform mixing SiO 2 powder and the alpha-silicon nitride powders of 40wt% and 60wt%, the mixed powder gross weight is 50 g, mode with its rotary integral quartz glass crucibles makes powder be evenly distributed on the first silicon oxynitride mixolimnion surface again, and sinters it into second silicon oxynitride mixolimnion with the pressure of 50 handkerchiefs and 1900 ℃ temperature; After electric arc electricity slurry reactor shifts out crucible, after treating that the quartz glass crucibles temperature descends, again SiO 2 powder and alpha-silicon nitride powders are repeated above-mentioned steps with the ratio (gross weight is all 50 g) of 30wt% and 70wt%, 20wt% and 80wt% and 10wt% and 90wt% afterwards and in regular turn the mode of rotary integral quartz glass crucibles make powder be uniformly distributed in the inboard and sintering of crucible and storehouse forms four second silicon oxynitride mixolimnions; After electric arc electricity slurry reactor shifts out crucible, after treating that the quartz glass crucibles temperature descends, afterwards again with the alpha-silicon nitride powders (gross weight is 50 g) of 100wt%, insert on this second silicon oxynitride mixolimnion surface, sinter it into silicon nitride layer in the mode of rotary integral quartz glass crucibles and with the pressure of 50 handkerchiefs and 1900 ℃ temperature.The total thickness of the first silicon oxynitride mixolimnion of finishing, the second silicon oxynitride mixolimnion and silicon nitride layer etc. is about 20 μ m.
Therefore the silicon oxynitride protective layer of present embodiment is made up of the first silicon oxynitride mixolimnion and four layer of second silicon oxynitride mixolimnion of five layers.
The present invention can be applicable to various quartz glass crucibles bodies, and can be by the amount of adjusting silicon nitride and/or silicon-dioxide control thickness, and reduce the amount of silicon-dioxide gradually with this, and slowly increase the amount of silicon nitride, can make the silicon oxide layer that is obtained more firmly combine, and increase the work-ing life of quartz glass crucibles with the quartz glass crucibles body.
Claims (10)
1. manufacture method with quartz glass crucibles of protective layer, it comprises:
One quartz glass crucibles body is provided;
Form at least one first silicon oxynitride mixolimnion in the inboard of this quartz glass crucibles body;
On this first silicon oxynitride mixolimnion, form at least one second silicon oxynitride mixolimnion again;
Form a silicon nitride layer in this second silicon oxynitride mixolimnion again, this the first silicon oxynitride mixolimnion and the second silicon oxynitride mixolimnion all are made up of silicon-dioxide and silicon nitride, wherein the silicon nitride of this second silicon oxynitride mixolimnion ratio that accounts for the second silicon oxynitride mixolimnion is many than the ratio that the silicon nitride of the first silicon oxynitride mixolimnion accounts for the first silicon oxynitride mixolimnion, and this silicon nitride layer is made up of silicon nitride.
2. the manufacture method with quartz glass crucibles of protective layer as claimed in claim 1, wherein the dioxide-containing silica of this first silicon oxynitride mixolimnion is less than the 100wt% of the whole first silicon oxynitride mixolimnion, and more than or equal to 50wt%, and the content of silicon nitride is the 0wt% greater than the whole first silicon oxynitride mixolimnion, and is less than or equal to 50wt%; The dioxide-containing silica of this second silicon oxynitride mixolimnion is less than the 50wt% of the whole first silicon oxynitride mixolimnion, and greater than 0wt%, and the content of silicon nitride is the 50wt% greater than the whole first silicon oxynitride mixolimnion, and less than 100wt%.
3. the manufacture method with quartz glass crucibles of protective layer as claimed in claim 1, wherein the material of this silicon-dioxide and silicon nitride is all the particle of 5～500 μ m.
4. the manufacture method with quartz glass crucibles of protective layer as claimed in claim 2, wherein the material of this silicon-dioxide and silicon nitride is all the particle of 5～500 μ m.
5. as each described manufacture method in the claim 1 to 4 with quartz glass crucibles of protective layer; wherein form this at least one first silicon oxynitride mixolimnion, this at least one second silicon oxynitride mixolimnion and this silicon nitride layer in the agglomerating mode in the inboard of this quartz glass crucibles body; and this agglomerating pressure is 20～100 handkerchiefs, and the agglomerating temperature is 1800～2000 ℃.
6. as each described manufacture method in the claim 1 to 4 with quartz glass crucibles of protective layer; wherein form this at least one first silicon oxynitride mixolimnion, this at least one second silicon oxynitride mixolimnion and this silicon nitride layer in the agglomerating mode in the inboard of this quartz glass crucibles body; and this agglomerating pressure is 50 handkerchiefs, and temperature is 1900 ℃.
7. quartz glass crucibles with protective layer, it is with made as each described manufacture method in the claim 1 to 6.
8. quartz glass crucibles with protective layer, it comprises:
One quartz glass crucibles body; And
One silicon oxynitride protective layer, it is formed on this quartz glass crucibles body inboard, and this silicon oxynitride protective layer has the cumulative silicon nitride and the ratio of silicon-dioxide from a side that contacts this quartz glass crucibles body towards other side;
One silicon nitride layer, it is arranged at the in addition side of this silicon oxynitride protective layer noncontact in this quartz glass crucibles body.
9. the quartz glass crucibles with protective layer as claimed in claim 8, wherein this silicon oxynitride protective layer comprises at least one first silicon oxynitride mixolimnion of the inboard that is formed on this quartz glass crucibles body and at least one second silicon oxynitride mixolimnion that is formed on the surface of this first silicon oxynitride mixolimnion; Wherein the dioxide-containing silica of this first silicon oxynitride mixolimnion is less than the 100wt% of the whole first silicon oxynitride mixolimnion, and more than or equal to 50wt%, and the content of silicon nitride is the 0wt% greater than the whole first silicon oxynitride mixolimnion, and is less than or equal to 50wt%; The dioxide-containing silica of this second silicon oxynitride mixolimnion is less than the 50wt% of the whole second silicon oxynitride mixolimnion, and greater than 0wt%, and the content of silicon nitride is the 50wt% greater than the whole second silicon oxynitride mixolimnion, and less than 100wt%, and the material of this silicon-dioxide and silicon nitride is all the particle of 5～500 μ m.
10. the quartz glass crucibles with protective layer as claimed in claim 8; wherein this silicon oxynitride protective layer is formed at least one first silicon oxynitride mixolimnion of inboard of this quartz glass crucibles body by this and at least one second silicon oxynitride mixolimnion on this surface that is formed on this first silicon oxynitride mixolimnion is formed, and the material of this silicon-dioxide and silicon nitride is all the particle of 5～500 μ m.
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| CN107916451A (en) * | 2017-12-15 | 2018-04-17 | 江苏润弛太阳能材料科技有限公司 | One kind casting polysilicon exempts to spray crucible |
| CN108046846A (en) * | 2017-12-15 | 2018-05-18 | 江苏润弛太阳能材料科技有限公司 | A kind of casting polysilicon exempts to spray crucible coating layer and preparation method thereof |
| CN114436506A (en) * | 2021-12-27 | 2022-05-06 | 深圳市众诚达应用材料科技有限公司 | Glass powder smelting method |
| CN114436506B (en) * | 2021-12-27 | 2023-11-24 | 深圳众诚达应用材料股份有限公司 | Glass powder smelting method |
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