CN102358953B - A kind ofly reduce crucible of sticky crucible and preparation method thereof - Google Patents
A kind ofly reduce crucible of sticky crucible and preparation method thereof Download PDFInfo
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- CN102358953B CN102358953B CN201110300886.8A CN201110300886A CN102358953B CN 102358953 B CN102358953 B CN 102358953B CN 201110300886 A CN201110300886 A CN 201110300886A CN 102358953 B CN102358953 B CN 102358953B
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Abstract
The invention provides and a kind ofly reduce crucible of sticky crucible and preparation method thereof.Crucible of the present invention comprises: body and silicon nitride layer, the sidewall that body comprises base and upwards extended by base, base and sidewall surround a receiving space jointly, silicon nitride layer is attached to the one side of body sidewall towards receiving space, body sidewall is being provided with slip-off preventing layer in one week apart from the position between body base first height and the second height along body sidewall, second height is higher than the first height, and silicon nitride layer is attached to body sidewall by slip-off preventing layer.Product of the present invention can reduce the generation of sticky crucible phenomenon significantly, thus improves the quality of silicon ingot.The inventive method is rationally easy, and by the method for silicon nitride layer Integral upset in hinge structure, the present invention effectively controls production cost, is suitable for large-scale industrial production and use.
Description
Technical field
The present invention relates to field of polycrystalline silicon ingot, particularly relate to and a kind ofly reduce crucible of sticky crucible and preparation method thereof.
Background technology
When polycrystalline furnace ingot casting, usually adopt ceramic crucible or quartz crucible to carry out splendid attire molten silicon liquid, molten silicon liquid is cooled in crucible, anneals and crystallization.But the main component silicon-dioxide of crucible body can with the silicon generation chemical reaction in molten silicon liquid, sticky crucible phenomenon is caused to occur, cause demoulding difficulty even silicon ingot and crucible break, and in the product of related chemistry reaction and crucible body, the impurity that exists will pollute molten silicon liquid.Therefore, most crucible body 91 inner side-walls is attached with one deck silicon nitride layer 92 as protective layer (as depicted in figs. 1 and 2), contacts with the direct of crucible body sidewall in order to cut off molten silicon liquid.
Silicon nitride layer is attached to crucible body sidewall by the slurry of beta-silicon nitride powder and solvent to form.The intensity of silicon nitride layer is not high, even be attached to the silicon nitride layer of crucible body sidewall by high-temperature roasting, also usually in view of following reason is peeled off, sticky crucible phenomenon is caused often to occur: needed for (1) ingot casting process, furnace temperature is higher and consuming time longer, air pressure is low, and silicon nitride layer easily decomposes; (2) flowing of molten silicon liquid constantly causes silicon nitride layer and washes away and the External Force Acting such as erosion, and silicon nitride layer easily peels off; (3) the other factors effect such as impurity.
At present, the general way increasing spraying silicon nitride layer thickness that adopts prevents silicon nitride layer from peeling off completely.But highly purified silicon nitride is expensive, limited source, the method is not suitable for large-scale industrial production and use.
Summary of the invention
For solving the problem, the present invention aims to provide and a kind ofly reduces crucible of sticky crucible and preparation method thereof.Product of the present invention can reduce the generation of sticky crucible phenomenon significantly, thus improves the quality of silicon ingot.The inventive method is rationally easy, by the method for silicon nitride layer Integral upset in hinge structure, effectively can control production cost, be suitable for large-scale industrial production and use.
On the one hand, the invention provides a kind of crucible reducing sticky crucible, comprise: body and silicon nitride layer, the sidewall that body comprises base and upwards extended by base, base and sidewall surround a receiving space jointly, silicon nitride layer is attached to the one side of body sidewall towards receiving space, wherein, body sidewall is being provided with slip-off preventing layer in one week apart from the position between body base first height and the second height along body sidewall, second height is higher than the first height, and silicon nitride layer is attached to body sidewall by slip-off preventing layer.
Operationally, in crucible, the molten silicon liquid (liquid phase) of splendid attire expands because crystallisation process volume becomes, and causes liquid level to rise.Applicant finds, in polycrystalline furnace ingot casting process, the sticky crucible phenomenon of more than 90% all appear at crucible body sidewall (solid phase), the molten silicon liquid (liquid phase) held and place, molten silicon liquid overhead gas (gas phase) three-phase boundary for body sidewall on region, therefore the present invention is made improvements this situation targetedly by calculating first height and second setting position highly.Particularly, the molten silicon liquid liquid level that crucible holds is the first height apart from the height of crucible body base, and when molten silicon liquid all changes solid-state silicon ingot into, silicon ingot upper surface is the second height apart from the height of crucible body base.
For the most widely used 840 crucibles (internal diameter 840mm × 840mm) at present, calculate with 400kg silicon material, in 840 crucibles, molten silicon liquid liquid level is apart from crucible body base height 227mm (i.e. the first height), when molten silicon liquid all becomes solid-state silicon ingot, silicon ingot upper surface is 244mm (the second height) apart from crucible body base height, in this situation, the setting position of slip-off preventing layer is apart from the region that crucible body base height is 227mm ~ 244mm on body sidewall.Calculate with 450kg silicon material, in same crucible, molten silicon liquid liquid level is apart from crucible body base height 255mm, when molten silicon liquid all becomes solid-state silicon ingot, silicon ingot upper surface is 273mm apart from crucible body base height, in this case, three-phase junction region is apart from the region that crucible body base height is 255mm ~ 273mm on crucible wall.In view of silicon material tap density difference to some extent, when 840 crucibles are used for work fill silicon material weight often within 400kg ~ 450kg scope not etc., therefore, preferably, crucible is 840 crucibles, and the position between the first height and the second height is that body sidewall is in the position apart from body base 227mm ~ 273mm.
Position between distance body base first height and the second height, silicon nitride layer is attached to body sidewall by slip-off preventing layer, is formed in case stratum disjunction is sandwich form.Outside this region, silicon nitride layer is directly attached on body sidewall.
Preferably, slip-off preventing layer is that body sidewall is through the uneven surface roughly ground or obtain after inlaying particle projection.In this region, silicon nitride layer and base side wall surface roughness are strengthened, improve body surface contacting face to amass, thus strengthen the sticking power of silicon nitride layer and the position of body sidewall between distance body base first height and the second height, improve the shock resistance of silicon nitride layer simultaneously.
Also preferably, slip-off preventing layer is inorganic bond oxidant layer or organic binder layer.Inorganic bond oxidant layer and organic binder layer all firmly can be combined with crucible body sidewall, again can with silicon nitride layer stable bond, thus strengthen the sticking power of silicon nitride layer and the position of body sidewall between distance body base first height and the second height, improve the shock resistance of silicon nitride layer simultaneously.More preferably, mineral binder bond is colloided silica, and organic binder bond is selected from one or more in polyoxyethylene glycol, polyvinyl alcohol, polycarbonate, epoxide, carboxymethyl cellulose.Inorganic bond oxidant layer or organic binder layer can be obtained by spraying.
The present invention has made improvement for the structure of crucible specific region " apart from the position between body base first height and the second height " first, improve the characteristic of this region crucible targetedly, namely enhance the sticking power of this region silicon nitride layer and body sidewall, decrease silicon nitride layer and decompose; Enhance silicon nitride opposing molten silicon liquid to flow the ability with erosion action of washing away brought, decrease peeling off of silicon nitride layer, thus significantly reduce the generation of sticky crucible phenomenon.
On the other hand, the invention provides a kind of preparation method reducing the crucible of sticky crucible, comprise the following steps: get crucible body, within one week, slip-off preventing layer is being provided with apart from the position between body base first height and the second height along body sidewall by the method roughly grinding, inlay particle projection or spraying, second height, higher than the first height, is being provided with the body sidewall attachment silicon nitride layer of slip-off preventing layer subsequently.
Preferably, crucible is 840 crucibles, and the position between the first height and the second height is that body sidewall is in the position apart from body base 227mm ~ 273mm.
Coarse base side wall surface can be obtained as slip-off preventing layer by roughly grinding or inlaying particle projection.After adhering to silicon nitride layer in this region, silicon nitride layer and base side wall surface roughness are strengthened, and the body surface contacting face between them is long-pending to be increased, thus strengthens the sticking power of this region silicon nitride layer and body sidewall, improves the shock resistance of silicon nitride layer simultaneously.
Inorganic bond oxidant layer or organic binder layer can be obtained as slip-off preventing layer by spraying.Inorganic bond oxidant layer and organic binder layer all firmly can be combined with body sidewall, again can with silicon nitride layer stable bond, thus strengthen the sticking power of silicon nitride layer and the position of body sidewall between distance body base first height and the second height, improve the shock resistance of silicon nitride layer simultaneously.More preferably, mineral binder bond is colloided silica, and organic binder bond is selected from one or more in polyoxyethylene glycol, polyvinyl alcohol, polycarbonate, epoxide, carboxymethyl cellulose.
The inventive method has carried out specific process for crucible specific region " apart from the position between body base first height and the second height ".The inventive method is rationally easy, and by the method for silicon nitride layer Integral upset in hinge structure, the property of the present invention is directed to is strong, effectively controls production cost, is suitable for large-scale industrial production and use.
Provided by the inventionly a kind ofly reduce crucible of sticky crucible and preparation method thereof, there is following beneficial effect:
(1) product of the present invention is by arranging slip-off preventing layer pointedly, enhances the sticking power of silicon nitride layer and the position of crucible body sidewall between distance body base first height and the second height, decreases silicon nitride layer and decompose; Enhance silicon nitride opposing molten silicon liquid to flow the ability with erosion action of washing away brought, decrease peeling off of silicon nitride layer; Thus significantly reduce the generation of sticky crucible phenomenon, improve the quality of silicon ingot;
(2) the inventive method is rationally easy, and by the method for silicon nitride layer Integral upset in hinge structure, the present invention effectively controls production cost, is suitable for large-scale industrial production and use.
Accompanying drawing explanation
Fig. 1 is the structural representation of common crucible;
Fig. 2 is the local section structural representation of common crucible;
Fig. 3 is the structural representation of crucible of the present invention;
Fig. 4 is three-phase position regional change scope schematic diagram;
Fig. 5 is the local section structural representation A of crucible of the present invention;
Fig. 6 is the local section structural representation B of crucible of the present invention;
Fig. 7 is the local section structural representation C of crucible of the present invention;
Embodiment
The following stated is the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications are also considered as protection scope of the present invention.
As shown in Figure 3, the invention provides a kind of crucible reducing sticky crucible, comprise: body 1 and silicon nitride layer 2, the sidewall that body 1 comprises base and upwards extended by base, base and sidewall surround a receiving space jointly, silicon nitride layer 2 is attached to the one side of body 1 sidewall towards receiving space, wherein, body 1 sidewall is being provided with slip-off preventing layer 3 in one week apart from the position between body 1 base first height and the second height along body 1 sidewall, second height is higher than the first height, and silicon nitride layer 2 is attached to body 1 sidewall by slip-off preventing layer 3.
As shown in Figure 4, for the most widely used 840 crucibles (internal diameter 840mm × 840mm) at present, usual feeding quantity, all within the scope of 400 ~ 450kg, calculates thus and learns that the position between the first height and the second height is that body sidewall is in the position apart from body base 227mm ~ 273mm.
Embodiment one
A kind of 840 crucibles (internal diameter 840mm × 840mm) reducing sticky crucible, comprise: body 1 and silicon nitride layer 2, the sidewall that body 1 comprises base and upwards extended by base, base and sidewall surround a receiving space jointly, silicon nitride layer 2 is attached to the one side of body 1 sidewall towards receiving space, wherein, body 1 sidewall is being provided with slip-off preventing layer 31 in one week apart from the position between body 1 base 227mm ~ 273mm along body 1 sidewall, and silicon nitride layer 2 is attached to body 1 sidewall by slip-off preventing layer 31.Slip-off preventing layer 31 is the uneven surface (as shown in Figure 5) that body 1 sidewall obtains after corase grind, in order to strengthen the sticking power in this region between silicon nitride layer 2 and body 1 sidewall.
Embodiment two
A kind of 840 crucibles (internal diameter 840mm × 840mm) reducing sticky crucible, structure is with embodiment one, and difference is only that slip-off preventing layer 32 is the uneven surface (as shown in Figure 6) that body 1 sidewall obtains after inlaying particle projection.
Embodiment three
A kind of 840 crucibles (internal diameter 840mm × 840mm) reducing sticky crucible, structure is with embodiment one, and difference is only that slip-off preventing layer 33 is colloided silica (inorganic bond oxidant layer) (as shown in Figure 7).
Embodiment four
A kind of 840 crucibles (internal diameter 840mm × 840mm) reducing sticky crucible, structure is with embodiment one, and difference is only that slip-off preventing layer is polyoxyethylene glycol and carboxymethyl cellulose gum state silicon oxide (organic binder layer).
Embodiment five
A kind of preparation method reducing 840 crucibles (internal diameter 840mm × 840mm) of sticky crucible, comprise the following steps: get crucible body, one week be provided with slip-off preventing layer apart from the position between body base 227mm ~ 273mm along body sidewall by the method for spraying, slip-off preventing layer is polyoxyethylene glycol and carboxymethyl cellulose gum state silicon oxide (organic binder layer).Be provided with the method attachment silicon nitride layer of body sidewall by spraying of slip-off preventing layer subsequently.
Claims (5)
1. one kind is reduced the crucible of sticky crucible, comprise: body and silicon nitride layer, the sidewall that body comprises base and upwards extended by base, base and sidewall surround a receiving space jointly, silicon nitride layer is attached to the one side of body sidewall towards receiving space, it is characterized in that, body sidewall is being provided with slip-off preventing layer in one week apart from the position between body base first height and the second height along body sidewall, second height is higher than the first height, silicon nitride layer is attached to body sidewall by slip-off preventing layer, described crucible is 840 crucibles, position between described first height and the second height is that body sidewall is in the position apart from body base 227mm ~ 273mm.
2. crucible as claimed in claim 1, is characterized in that, described slip-off preventing layer is that body sidewall is through the uneven surface roughly ground or obtain after inlaying particle projection.
3. crucible as claimed in claim 1, it is characterized in that, described slip-off preventing layer is inorganic bond oxidant layer or organic binder layer.
4. crucible as claimed in claim 3, it is characterized in that, described mineral binder bond is colloided silica, and organic binder bond is selected from one or more in polyoxyethylene glycol, polyvinyl alcohol, polycarbonate, epoxide, carboxymethyl cellulose.
5. one kind is reduced the preparation method of the crucible of sticky crucible, it is characterized in that, comprise the following steps: get crucible body, within one week, slip-off preventing layer is being provided with apart from the position between body base first height and the second height along body sidewall by the method roughly grinding, inlay particle projection or spraying, second height is higher than the first height, be provided with the body sidewall attachment silicon nitride layer of slip-off preventing layer subsequently, described crucible is 840 crucibles, and the position between described first height and the second height is that body sidewall is in the position apart from body base 227mm ~ 273mm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201110300886.8A CN102358953B (en) | 2011-09-28 | 2011-09-28 | A kind ofly reduce crucible of sticky crucible and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201110300886.8A CN102358953B (en) | 2011-09-28 | 2011-09-28 | A kind ofly reduce crucible of sticky crucible and preparation method thereof |
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| CN102358953A CN102358953A (en) | 2012-02-22 |
| CN102358953B true CN102358953B (en) | 2015-12-09 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP6743753B2 (en) * | 2017-04-27 | 2020-08-19 | 株式会社Sumco | Silicon single crystal pulling method |
| CN109111102A (en) * | 2018-11-02 | 2019-01-01 | 宁夏富乐德石英材料有限公司 | A kind of semiconductor grade silica crucible and its manufacturing method |
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| CN1683101A (en) * | 2004-04-16 | 2005-10-19 | Tdk株式会社 | Method of manufacturing nickel powder, apparatus for manufacturing nickel powder, and crucible for manufacturing nickel powder |
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| JPS60141696A (en) * | 1983-12-28 | 1985-07-26 | Hitachi Cable Ltd | Device for growing single crystal |
| JPH0597571A (en) * | 1991-06-13 | 1993-04-20 | Toshiba Ceramics Co Ltd | Crucible for pulling up silicon single crystal |
| JP4798714B2 (en) * | 2007-03-28 | 2011-10-19 | コバレントマテリアル株式会社 | Silica glass crucible for pulling silicon single crystals |
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| CN86100240A (en) * | 1986-01-07 | 1987-07-22 | 中国有色金属工业总公司昆明贵金属研究所 | Pottery-platinum composite crucible and manufacture method thereof |
| CN1742120A (en) * | 2002-12-06 | 2006-03-01 | 维苏威法兰西股份有限公司 | Vessel for holding silicon and method of producing the same |
| CN1683101A (en) * | 2004-04-16 | 2005-10-19 | Tdk株式会社 | Method of manufacturing nickel powder, apparatus for manufacturing nickel powder, and crucible for manufacturing nickel powder |
| CN101184595A (en) * | 2005-05-23 | 2008-05-21 | 住友重机械工业株式会社 | Disc molding mold, mirror-surface disc, and method for producing mold for disc molding |
| CN101278078A (en) * | 2005-10-06 | 2008-10-01 | 维苏威克鲁斯布公司 | Crucible for crystallizing silicon and producing mtheod thereof |
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