CN105256370A - Method for preparing high-purity crucible provided with smooth inner surface - Google Patents
Method for preparing high-purity crucible provided with smooth inner surface Download PDFInfo
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- CN105256370A CN105256370A CN201510704655.1A CN201510704655A CN105256370A CN 105256370 A CN105256370 A CN 105256370A CN 201510704655 A CN201510704655 A CN 201510704655A CN 105256370 A CN105256370 A CN 105256370A
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Abstract
The invention relates to a method for preparing a high-purity crucible provided with a smooth inner surface. The method includes the steps that 1, after high-purity single crystal raw sand, high-purity polycrystalline cooked sand and a binding agent A are evenly mixed according to a certain proportion, the mixture is evenly arranged on the inner wall of a polycrystalline crucible in a coating mode, and a high-purity coating is obtained; 2, the temperature of the polycrystalline crucible coated with the high-purity coating is rapidly raised to 600-800 DEG C through a high-temperature sintering furnace, and temperature preservation is conducted for 1 hour; 3, after high-purity silicon nitride powder and a binding agent B are evenly mixed, the surface of the high-purity coating of the high-purity crucible processed in step 2 is coated with a high-purity silicon nitride coating in a roller coating mode, after ingot unloading is conducted through a silicon ingot cast by the crucible, the surface of the silicon ingot is smooth, no crucible sticking and cracking phenomena exist, and the crucible sticking rate can be controlled within 5%.; the width of the black edge of a crystal brick on the contact face of the polycrystalline silicon ingot and the crucible is greatly lowered compared with an ordinary cast ingot, and the width of the black edge of the crystal brick on the side edge of the cast ingot can be greatly lowered to be 3-4 mm per edge from 16-18 mm per edge of a normal crystal brick.
Description
Technical field
The present invention relates to a kind of preparation method with the high-purity crucible of wall of slippery inner surface, belong to polysilicon casting field.
Background technology
At present, the directional solidification system that the preparation method of polycrystal silicon ingot mainly utilizes GTSolar to provide is prepared, and the method generally includes the steps such as heating, fusing, long crystalline substance, annealing and cooling.Solidifying in long brilliant process, by controlling head temperature and side stay-warm case aperture, molten silicon liquid is made to obtain enough condensate depression solidification and crystallizations in crucible bottom.But an important auxiliary material---the polycrystalline cast ingot quartz crucible of ingot casting use at present, due to the purity of self relatively low (purity is about 4N only), cause in ingot casting process, have the impurity of a large amount of crucible inside to enter into polycrystal silicon ingot by thermodiffusion, the brilliant brick contacted with crucible wall is made easily to form impurity enriched district, referred to as " black surround ", the further lifting of the polycrystal silicon ingot efficiency greatly affected, is more and more difficult to meet the demand of market for the high-efficiency polycrystalline silicon chip of low impurity concentration;
Low for current common crucible purity, a large amount of harmful metal impurity is had easily to enter silicon ingot by thermodiffusion in ingot casting process, the overall purity drop of silicon ingot, cause the problem that photoelectric transformation efficiency reduces, technician develops two kinds of different schemes to eliminate the impact of crucible diffusion of contaminants on ingot casting: a kind of for by increasing crucible size, increase the thickness removing edge skin material when removing edge skin material and reach the object reducing black surround width, specifically refer to and the size of the 878mm of current normal crucible is risen to 890mm, reduce brilliant brick black surround width, this scheme can make black surround width reduce the brilliant brick of 5 ~ 6mm/, but because crucible footpath increases, ingot casting applicable part silicon material utilization ratio is significantly reduced, greatly improve ingot casting cost, another kind of scheme is brush one deck glass sand in crucible inside, diffusion of contaminants is stoped by setting up diffusion of contaminants barrier layer, the black surround width of brilliant brick effectively can be reduced by this scheme, generally the black surround width of about the 18mm of normal brilliant brick can be reduced to about 6 ~ 8mm, and this case does not change due to crucible size, on silicon material utilization ratio substantially without impact, but the high-purity coating due to current high-purity crucible surface process is the mode by brushing brushes at crucible surface, crucible internal walls roughness is caused significantly to promote, the silicon nitride as ingot casting sealing coat is made not easily to adhere to crucible surface, utilize silicon ingot that high-purity crucible is cast to glue crucible crackle abnormal conditions significantly to promote, cause larger windfall loss, improve ingot casting cost, in addition because crucible wall roughness promotes, cause crystal sidewall forming core probability in ingot casting process significantly to promote, the inner dislocation of silicon ingot is increased, the further lifting of the silicon ingot photoelectric transformation efficiency greatly limited.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of preparation method with the high-purity crucible of wall of slippery inner surface, utilizes silicon ingot that this crucible is cast to unload silicon ingot smooth surface after ingot, and without sticky crucible seminess, sticky crucible rate can be controlled within 5 ‰; Cast the brilliant brick of polycrystal silicon ingot and crucible contact surface black surround width compare common ingot casting and significantly reduce, ingot casting side brilliant brick black surround width can significantly reduce to 3 ~ 4mm/ limit by 16 ~ 18mm/ limit of normal brilliant brick.
For solving the problems of the technologies described above, technical scheme of the present invention is:
Have a preparation method for the high-purity crucible of wall of slippery inner surface, its preparation method is:
1), after first high purity single crystal greensand, the ripe sand of High Purity Polycrystalline and binding agent A being mixed according to a certain percentage, utilize the mode of brushing to brush uniformly and obtain high-purity coating on polycrystalline crucible internal walls, the thickness of described high-purity coating is 2 ~ 3mm; Described high-purity coating with the downward 10cm place of crucible top margin for starting point, until whole crucible basal edge region;
2) the polycrystalline crucible of brushing good high-purity coating is rapidly heated to 600 ~ 800 DEG C through high temperature sintering furnace, and is incubated 1h;
3), after being mixed with binding agent B by high purity silicon nitride silica flour, the mode of roller coating is utilized through step 2) high-purity crucible high-purity coatingsurface roller coating one deck high purity silicon nitride silicon coating after process, described high purity silicon nitride coat-thickness is 60 ~ 80um.
Above-mentioned a kind of preparation method with the high-purity crucible of wall of slippery inner surface, wherein, described high purity single crystal greensand: the ripe sand of High Purity Polycrystalline: the weight ratio of binding agent A is 1:1:(4 ~ 6); Described high purity single crystal greensand purity >=5.5N, granularity is 400 ~ 500 orders, the ripe sand purity >=5N of described High Purity Polycrystalline, granularity is 400 ~ 600 orders, described binding agent A is one or both the mixture in high-purity silicasol or pure water, the solid content of described high-purity silicasol is 40 ~ 41%, and particle diameter is 25 ~ 29nm.
Above-mentioned a kind of preparation method with the high-purity crucible of wall of slippery inner surface, wherein, described polycrystalline crucible outside diameter d 1 is 878 ~ 880mm, and internal diameter d2 is 838 ~ 840mm, and height h is 480mm, and self purity of polycrystalline crucible is 4N
Above-mentioned a kind of preparation method with the high-purity crucible of wall of slippery inner surface, wherein, described high temperature sintering furnace is microwave heating sintering oven.
Above-mentioned a kind of preparation method with the high-purity crucible of wall of slippery inner surface, wherein, the weight ratio that described high purity silicon nitride silica flour mixes with binding agent B is 1:3 ~ 1:5; Purity>=the 5N of described high purity silicon nitride, silicon nitride particle degree D
50between 1.3 ~ 3um; Described binding agent B is the mixture of pure water and high-purity silicasol, and the weight ratio of pure water and silicon sol is 1:6 ~ 1:8.
Beneficial effect of the present invention is:
1) the invention provides a kind of preparation method with high-purity crucible of slippery inner surface, utilize silicon ingot that this crucible is cast to unload silicon ingot smooth surface after ingot, indifference basic with common crucible, and substantially without sticky crucible seminess, sticky crucible rate can be controlled within 5 ‰;
2) a kind of high-purity crucible with slippery inner surface of the present invention is utilized, cast the brilliant brick of polycrystal silicon ingot and crucible contact surface black surround width compare common ingot casting and significantly reduce, utilize high-purity crucible institute of the present invention ingot casting side brilliant brick black surround width can significantly reduce to 3 ~ 4mm/ limit by 16 ~ 18mm/ limit of normal brilliant brick.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention.
Embodiment
Embodiment one
Have a preparation method for the high-purity crucible of wall of slippery inner surface, its preparation method is:
1) after first high purity single crystal greensand, the ripe sand of High Purity Polycrystalline and binding agent A being mixed according to a certain percentage, utilizing the mode of brushing to brush at external diameter d1 is uniformly 880mm, internal diameter d2 is 840mm, height h is 480mm, self purity be 4N polycrystalline crucible 1 inwall on high-purity coating 2, the thickness of described high-purity coating 2 is 2.5mm; Described high-purity coating with the downward 10cm place of crucible top margin for starting point, until whole crucible basal edge region, described high purity single crystal greensand: the ripe sand of High Purity Polycrystalline: the weight ratio of binding agent A is 1:1:5; Described high purity single crystal greensand purity is 5.5N, and granularity is 450 orders, and the ripe sand purity of described High Purity Polycrystalline is 5N, granularity is 500 orders, described binding agent A is that high-purity silicasol or pure water mix with the weight ratio of 1:3, and the solid content of described high-purity silicasol is 41%, and particle diameter is 26nm;
2) by brushing the polycrystalline crucible 1 of good high-purity coating 2 through microwave heating sintering oven, from room temperature to 700 DEG C in 2.5h, and naturally cooling after being incubated 1h;
3) after high purity silicon nitride silica flour being mixed with binding agent B, utilize the mode of roller coating through step 2) the high-purity coating of high-purity crucible 2 surperficial roller coating one deck high purity silicon nitride silicon coating 3 after process, described high purity silicon nitride coat-thickness is 70um, and the weight ratio that described high purity silicon nitride silica flour mixes with binding agent B is 1:4; The purity of described high purity silicon nitride is 5N, silicon nitride particle degree D
50for 2um; Described binding agent B is the mixture of pure water and high-purity silicasol, and the weight ratio of pure water and silicon sol is 1:7.
Embodiment two
Have a preparation method for the high-purity crucible of wall of slippery inner surface, its preparation method is:
1) after first high purity single crystal greensand, the ripe sand of High Purity Polycrystalline and binding agent A being mixed according to a certain percentage, utilizing the mode of brushing to brush at external diameter d1 is uniformly 880mm, internal diameter d2 is 840mm, height h is 480mm, self purity be 4N polycrystalline crucible 1 inwall on high-purity coating 2, the thickness of described high-purity coating 2 is 3mm; Described high-purity coating with the downward 10cm place of crucible top margin for starting point, until whole crucible basal edge region, described high purity single crystal greensand: the ripe sand of High Purity Polycrystalline: the weight ratio of binding agent A is 1:1:6; Described high purity single crystal greensand purity is 5.5N, and granularity is 500 orders, and the ripe sand purity of described High Purity Polycrystalline is 5N, and granularity is 500 orders, and described binding agent A is high-purity silicasol, and the solid content of described high-purity silicasol is 41%, and particle diameter is 26nm;
2) by brushing the polycrystalline crucible 1 of good high-purity coating 2 through microwave heating sintering oven, from room temperature to 600 DEG C in 2h, and naturally cooling after being incubated 1h;
3) after high purity silicon nitride silica flour being mixed with binding agent B, utilize the mode of roller coating through step 2) the high-purity coating of high-purity crucible 2 surperficial roller coating one deck high purity silicon nitride silicon coating 3 after process, described high purity silicon nitride silicon coating 3 thickness is 80um, and the weight ratio that described high purity silicon nitride silica flour mixes with binding agent B is 1:5; The purity of described high purity silicon nitride is 5N, silicon nitride particle degree D
50for 2.5um; Described binding agent B is the mixture of pure water and high-purity silicasol, and the weight ratio of pure water and silicon sol is 1:8.
The invention provides a kind of preparation method with high-purity crucible of slippery inner surface, utilize silicon ingot that this crucible is cast to unload silicon ingot smooth surface after ingot, indifference basic with common crucible, and substantially without sticky crucible seminess, sticky crucible rate can be controlled within 5 ‰;
Utilize a kind of high-purity crucible with slippery inner surface of the present invention, cast the brilliant brick of polycrystal silicon ingot and crucible contact surface black surround width compare common ingot casting and significantly reduce, utilize high-purity crucible institute of the present invention ingot casting side brilliant brick black surround width can significantly reduce to 3 ~ 4mm/ limit by 16 ~ 18mm/ limit of normal brilliant brick.
Here description of the invention and application is illustrative, not wants by scope restriction of the present invention in the above-described embodiments, and therefore, the present invention is not by the restriction of the present embodiment, and the technical scheme that any employing equivalence replacement obtains is all in the scope of protection of the invention.
Claims (5)
1. have a preparation method for the high-purity crucible of wall of slippery inner surface, it is characterized by, its preparation method is:
1), after first high purity single crystal greensand, the ripe sand of High Purity Polycrystalline and binding agent A being mixed according to a certain percentage, utilize the mode of brushing to brush uniformly and obtain high-purity coating on polycrystalline crucible internal walls, the thickness of described high-purity coating is 2 ~ 3mm; Described high-purity coating with the downward 10cm place of crucible top margin for starting point, until whole crucible basal edge region;
2) the polycrystalline crucible of brushing good high-purity coating is rapidly heated to 600 ~ 800 DEG C through high temperature sintering furnace, and is incubated 1h;
3), after being mixed with binding agent B by high purity silicon nitride silica flour, the mode of roller coating is utilized through step 2) high-purity crucible high-purity coatingsurface roller coating one deck high purity silicon nitride silicon coating after process, described high purity silicon nitride coat-thickness is 60 ~ 80um.
2. a kind of preparation method with the high-purity crucible of wall of slippery inner surface as claimed in claim 1, is characterized by, described high purity single crystal greensand: the ripe sand of High Purity Polycrystalline: the weight ratio of binding agent A is 1:1:(4 ~ 6); Described high purity single crystal greensand purity >=5.5N, granularity is 400 ~ 500 orders, the ripe sand purity >=5N of described High Purity Polycrystalline, granularity is 400 ~ 600 orders, described binding agent A is one or both the mixture in high-purity silicasol or pure water, the solid content of described high-purity silicasol is 40 ~ 41%, and particle diameter is 25 ~ 29nm.
3. a kind of preparation method with the high-purity crucible of wall of slippery inner surface as claimed in claim 1, it is characterized by, described polycrystalline crucible outside diameter d 1 is 878 ~ 880mm, and internal diameter d2 is 838 ~ 840mm, and height h is 480mm, and self purity of polycrystalline crucible is 4N.
4. a kind of preparation method with the high-purity crucible of wall of slippery inner surface as claimed in claim 1, it is characterized by, described high temperature sintering furnace is microwave heating sintering oven.
5. a kind of preparation method with the high-purity crucible of wall of slippery inner surface as claimed in claim 1, it is characterized by, the weight ratio that described high purity silicon nitride silica flour mixes with binding agent B is 1:3 ~ 1:5; Purity>=the 5N of described high purity silicon nitride, silicon nitride particle degree D
50between 1.3 ~ 3um; Described binding agent B is the mixture of pure water and high-purity silicasol, and the weight ratio of pure water and silicon sol is 1:6 ~ 1:8.
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Cited By (2)
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Application publication date: 20160120 |
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