CN105154971A - High-purity coating type polycrystalline silicon crucible and brushing method of coating of high-purity coating type polycrystalline silicon crucible - Google Patents
High-purity coating type polycrystalline silicon crucible and brushing method of coating of high-purity coating type polycrystalline silicon crucible Download PDFInfo
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Abstract
The invention relates to a high-purity coating type polycrystalline silicon crucible and a brushing method of a coating of the high-purity coating type polycrystalline silicon crucible. The high-purity coating type polycrystalline silicon crucible comprises a crucible body, wherein a plurality of pit or annular grooves are uniformly formed in the surface of the crucible body, and the surface of the crucible body is sequentially adhered with a first nitration layer, a second oxidization layer and a third nitration layer; the surface of the crucible body is brushed with the whey-state first nitration layer, powdery silicon oxide of the second oxidization layer is ejected to the surface of whey, vaporous silicon nitride is sprayed to the surface of the second oxidization layer until particles of the second oxidization layer are covered, and a smooth surface is formed on the third nitration layer. The high-purity coating type polycrystalline silicon crucible and the brushing method have the characteristics that the coating is strong in covering capacity and high in stability and isolation degree, and the crucible body is prevented from reacting during the preparation of polycrystalline silicon.
Description
Technical field
The present invention relates to manufacture of solar cells equipment technical field, be specifically related to the brushing method of a kind of high-purity coating type polysilicon crucible and coating thereof.
Background technology
As everyone knows, world today's supply of electric power is gradually nervous, and the utilization of photovoltaic technology can alleviate this situation effectively.Photovoltaic generation mainly contains monocrystalline, polycrystalline cell piece technology, and compared with monocrystalline, polycrystalline photovoltaic has that energy consumption is little, efficiency advantages of higher; In the same time, consume the same energy, polycrystalline output will be 6 ~ 7 times of monocrystalline, and thus polycrystalline found broad application in recent years.
In recent years, increasingly mature along with solar energy generation technology, solar cell obtains widespread use at numerous areas such as industry, agricultural and space flight.At present, according to the difference of material therefor, solar cell can be divided into: silicon solar cell, compound film solar cell and polymer multi-layer modified electrode solar cell, organic solar batteries and nano-crystalline solar battery.Wherein, silicon solar cell development is the most ripe, occupies an leading position in the application.Crystal silicon solar energy battery is divided into again monocrystaline silicon solar cell and polysilicon solar cell.Relative to monocrystaline silicon solar cell, polycrystal silicon cell solar cell preparation process is comparatively simple, has the advantages such as cost low energy is low, and therefore polysilicon solar cell application is comparatively extensive.
Crucible is the required equipment that polycrystalline silicon ingot casting is produced.At present, production of polysilicon mainly adopts quartz crucible, this is because silica source enriches, purity is high, and cheap.Although use quartz crucible to produce polycrystalline silicon ingot casting to contribute to reducing production cost, its defect existed is that the problem ftractureed easily appears in silicon ingot when cooling.This mainly because: the silicon dioxde reaction that the silicon of melting can be in contact with it, forms silicon monoxide and oxygen; Wherein, oxygen can pollute silicon, and silicon monoxide has volatility; And it also can form silicon carbide and carbon monoxide with the graphite member in stove, generate carbon monoxide then can with the pasc reaction of melting, form the carbide of volatile silicon monoxide, silicon carbide, metallic traces or doping agent, oxide compound and carbon, carbon can pollute silicon.Above-mentioned reaction between silicon-dioxide and molten silicon impels silicon to be attached on crucible.But because the thermal expansivity between silicon-dioxide and this bi-material of silicon is different, cause silicon ingot easily to ftracture when cooling.
In order to avoid silicon ingot ftractures when cooling, usually needing to use supercoat at inner surface of crucible, silicon-dioxide and molten silicon can be stoped thus to react, and then reducing silicon ingot pollution and cracking.This coating is sufficiently thick in stop silicon-dioxide and molten silicon to react, and must ensure that the high purity of this coating pollutes silicon to prevent the detrimental impurity in it.
Prior art has employing chemical Vapor deposition process to prepare silicon nitride coating, such as, discloses a kind of crucible silicon nitride coating prepared at 1250 DEG C by chemical vapour deposition in the United States Patent (USP) of the patent No. 4741925.And for example the patent No. is that the PCT of WO2004053207A1 patent discloses by plasma spraying silicon nitride coating.Although the problem that aforesaid method can prevent silicon nitride coating from coming off or peeling off, this method required equipment price costly and complicated operation.
In order to cost-saving, prior art mainly adopts silicon nitride as crucible coating layer.Current sun power industry uses comparatively general method to be mainly oxidized under controlled burnout cycle under the high temperature of 700 ~ 1450 DEG C by silicon nitride coating, thus makes to produce bonding between silicon nitride particle and between silicon nitride particle and quartz crucible.The defect of the method is that silicon nitride coating dust in thermal spray process is large, and local location easily has bubble, and calcining temperature is higher, and energy consumption is large.
Current in addition, for the crucible that polysilicon fusion-crystallization uses, all adopt in the industry high purity graphite material to make, self manufacturing cost is larger; And the polycrystalline silicon ingot casting that plumbago crucible crystallization goes out, its impurity content is higher, and effective recovery rate of silicon ingot is very low, and there is the defects such as result of use is undesirable, can not large-scale production and application with fashion, and therefore, polysilicon crucible has wide market outlook.
In prior art, usually can at surface-coated one deck silicon nitride coating of crucible.But the silicon nitride material of densification must liquid phase sintering under nitrogen protection atmosphere and hot environment; and size shrinks more than 10% than before sintering after usually fine and close silicon nitride material sintering; so the silicon nitride layer of quartz crucible surface coating is difficult to reach high fine and close degree, production requirement cannot be met.
Summary of the invention
The object of the invention is to overcome defect of the prior art, design a kind of high-purity coating type polysilicon crucible, make it have coating covering power strong, stability is high, has high-isolation, prevents crucible body from preparing in polysilicon process the feature participating in reacting.
For achieving the above object, the technical solution adopted in the present invention is:
A kind of high-purity coating type polysilicon crucible, comprise crucible body, several pits or annular recesses is evenly equipped with on described crucible surface originally, the first nitride layer, the second zone of oxidation and the 3rd nitride layer is attached with successively on the described surface being evenly equipped with several pits or annular recesses, this surface of described crucible is internal surface and the bead place, upper end of crucible, and the shape of cross section of described pit is the shape of cross section of Ω ring connected in star is dove-tail;
Described first nitride layer is by brushing mode, and by the silicon nitride coated of Mag in the crucible surface being originally evenly equipped with several pits or annular recesses, the coating thickness scope of described first nitride layer is 2 ~ 20mm;
Described second zone of oxidation is pulverous silicon oxide, and the first nitride layer sprayed pulverous silicon oxide in the Mag not yet condensed by spray regime is surperficial, and described second zone of oxidation forms particulate state on the surface of the first nitride layer;
Described 3rd nitride layer is vaporific silicon nitride, and by spraying method by the surface of vaporific silicon nitride spray finishing in the second zone of oxidation, until the particle of described second zone of oxidation is capped, described 3rd nitride layer forms shiny surface.
Wherein preferred technical scheme is, described first nitride layer comprises silicon nitride, hydrated barta and caking agent, described silicon nitride, hydrated barta and caking agent form the first nitride layer by brushing mode after adding deionized water and stirring formation Mag, the silicon oxide of described second zone of oxidation adopts lance ejection, the spray speed scope of described spray gun is 5 ~ 20km/h, is 20 ~ 100cm apart from the jet length scope of injected.
Preferred technical scheme also has, and described caking agent is the one in organosilane, silicic acid, polyvalent alcohol, polyvinyl alcohol and acrylate.
Preferred technical scheme also has, and the weight ratio of described silicon nitride, hydrated barta, caking agent and deionized water is 100:5 ~ 1:15 ~ 30:8 ~ 15.
Preferred technical scheme also has, and described second zone of oxidation is silicon oxide, and described silicon oxide is reacted by silicon nitride and hyperoxia agent to be made, and described hyperoxia agent is any one in hydrogen peroxide, ozone, the vitriol oil, nitric acid, potassiumchromate, potassium permanganate.
Preferred technical scheme also has further, and described polysilicon crucible body is a cuboid container, and the length range of described polysilicon crucible upper port is 2 ~ 3m, and width range is 0.5 ~ 1m.
Preferred technical scheme also has further, and the outer side wall of described crucible body is also covered with the first silicon nitride layer.
Another object of the present invention is, design a kind of brushing method of coating of high-purity coating type polysilicon crucible, it is strong that the coating after making it brush has coating covering power, and stability is high, there is high-isolation, prevent crucible body from preparing in polysilicon process the feature participating in reacting.
For achieving the above object, another technical scheme of the present invention is:
Based on a brushing method for the coating of above-mentioned high-purity coating type polysilicon crucible, comprise the following steps:
S1, polysilicon crucible body is processed into the surface being evenly equipped with several pits or annular recesses;
S2, be evenly equipped with first nitride layer of brushing Mag on surface of polysilicon crucible body of several pits or annular recesses, and making the first nitride layer be filled in several pits described or annular recesses;
S3, before the first nitride layer condensation of described Mag, in the second zone of oxidation of described first nitride layer surface jet particle shape;
S4 and then spray vaporific the 3rd nitride layer, until the 3rd vaporific nitride layer covers granular second zone of oxidation completely to granular second zone of oxidation surface;
S5, high temperature sintering, until the first nitride layer of Mag, the second zone of oxidation and the 3rd nitride layer condense completely and become an one-piece construction with polysilicon crucible body.
Wherein preferred technical scheme is that, in described step S2, described first nitride layer comprises silicon nitride, hydrated barta and caking agent, and described silicon nitride, hydrated barta and caking agent add deionized water and stirring and form Mag.
Preferred technical scheme also has, and in described step S3, described second zone of oxidation is granular silicon oxide, and the granular size scope of described silicon oxide is 2 ~ 10mm
2, described granular silicon oxide adopts lance ejection to the surface of the first nitride layer of Mag.
Preferred technical scheme also has, and in described step S4, is sprayed by described the 3rd vaporific nitride layer after covering the second zone of oxidation particle completely, then by rubber, the 3rd nitride layer above the second zone of oxidation particle is polished into smooth plane.
Preferred technical scheme also has, and in described step S5, described sintering range is 80 ~ 200 DEG C.
Advantage and the beneficial effect of high-purity coating type polysilicon crucible of the present invention are: preparation cost is low and coating covering power is strong, effectively prevent the sintering shrinkage of silicon nitride, stability is high, has high-isolation, preventing crucible body preparing participation reaction in polysilicon process, meeting production requirement.
In the first nitride layer of described high-purity coating type polysilicon crucible, the binding agent adopted is organosilane, silicic acid, polyvalent alcohol, polyvinyl alcohol or the acrylate that sticking temperature is lower, above-mentioned binding agent can reduce the temperature of subsequent calcination on the one hand, calcining temperature is reduced to 80 DEG C ~ 200 DEG C, reduces energy consumption thus; Improve slurry viscosity on the other hand, reduce the Dust Capacity produced in follow-up spraying process, ensure the HUMAN HEALTH of operator, reduce environmental pollution; In addition, it can also improve the cohesive strength of silicon nitride coating and crucible, improves the mechanical property of coating.Further, the present invention also controls the consumption of binding agent and silicon nitride.
In the first nitride layer, add hydrated barta, react with silicon and boron impurities wherein under high temperature, generate BOH gas, with SiO volatilization, thus the effect except boron can be played.
In addition, owing to being evenly equipped with several pits or annular recesses on crucible surface originally, and the shape of cross section that the shape of cross section of described pit is Ω ring connected in star is dove-tail.The throat structure that namely inner chamber is less compared with large port, so just can improve the adhesion strength on the first nitride layer and this surface of crucible further.
Accompanying drawing explanation
Fig. 1 is the local structure schematic diagram of the high-purity coating type polysilicon crucible of the present invention.
In figure: 1, crucible body; 2, pit; 3, the first nitride layer; 4, the second zone of oxidation; 5, the 3rd nitride layer.
Embodiment
Below in conjunction with drawings and Examples, the specific embodiment of the present invention is further described.Following examples only for technical scheme of the present invention is clearly described, and can not limit the scope of the invention with this.
Embodiment 1
As shown in Figure 1: the present invention is a kind of high-purity coating type polysilicon crucible, comprise crucible body 1, be evenly equipped with several pits 2 on this surface of 1 of described crucible, be attached with the first nitride layer 3, second zone of oxidation 4 and the 3rd nitride layer 5 successively on the described surface being evenly equipped with several pits 2;
Described first nitride layer 3 is by brushing mode, and by the silicon nitride coated of Mag in this 1 the surface of crucible being evenly equipped with several pits 2, the coating thickness scope of described first nitride layer 3 is 2mm;
Described second zone of oxidation 4 is pulverous silicon oxide, and the first nitride layer 3 sprayed pulverous silicon oxide in the Mag not yet condensed by spray regime is surperficial, and described second zone of oxidation 4 forms particulate state on the surface of the first nitride layer 3;
Described 3rd nitride layer 5 is vaporific silicon nitride, and by spraying method by the surface of vaporific silicon nitride spray finishing in the second zone of oxidation 4, until the particle of described second zone of oxidation 4 is capped, described 3rd nitride layer 5 forms shiny surface.
The preferred technical scheme of the present invention is, described first nitride layer 3 comprises silicon nitride, hydrated barta and caking agent, and described silicon nitride, hydrated barta and caking agent form the first nitride layer 3 by brushing mode after adding deionized water and stirring formation Mag.
The preferred embodiment of the invention also has, and described caking agent is organosilane.
The preferred embodiment of the invention also has, and the weight ratio of described silicon nitride, hydrated barta, caking agent and deionized water is 100:1:15:8.
The preferred embodiment of the invention also has, and described second zone of oxidation 4 is silicon oxide, and described silicon oxide is reacted by silicon nitride and hyperoxia agent to be made, and described hyperoxia agent is hydrogen peroxide.
Further preferred embodiment of the present invention also has, and the described silicon oxide of the 24 adopts lance ejection, and the spray speed scope of described spray gun is 5km/h, is 20cm apart from the jet length scope of injected.
The preferred embodiment of the invention also has, and this surface of 1 of described crucible is internal surface and the bead place, upper end of crucible.
Further preferred embodiment of the present invention also has, and the shape of cross section of described pit 2 is Ω shape.
Further preferred embodiment of the present invention also has, and described polysilicon crucible body 1 is a cuboid container, and the length range of described polysilicon crucible upper port is 2m, and width range is 0.5m.
Further preferred embodiment of the present invention also has, and the outer side wall of described crucible body 1 is also covered with the first silicon nitride layer 3.
Based on a brushing method for the coating of above-mentioned high-purity coating type polysilicon crucible, comprise the following steps:
S1, polysilicon crucible body is processed into the surface being evenly equipped with several pits or annular recesses;
S2, be evenly equipped with first nitride layer of brushing Mag on surface of polysilicon crucible body of several pits, and making the first nitride layer be filled in several pits described or annular recesses;
S3, before the first nitride layer condensation of described Mag, in the second zone of oxidation of described first nitride layer surface jet particle shape;
S4 and then spray vaporific the 3rd nitride layer, until the 3rd vaporific nitride layer covers granular second zone of oxidation completely to granular second zone of oxidation surface;
S5, high temperature sintering, until the first nitride layer of Mag, the second zone of oxidation and the 3rd nitride layer condense completely and become an one-piece construction with polysilicon crucible body.
The preferred embodiment of the invention is, in described step S2, described first nitride layer comprises silicon nitride, hydrated barta and caking agent, and described silicon nitride, hydrated barta and caking agent add deionized water and stirring and form Mag.
The preferred embodiment of the invention also has, and in described step S3, described second zone of oxidation is granular silicon oxide, and the granular size scope of described silicon oxide is 2mm
2, described granular silicon oxide adopts lance ejection to the surface of the first nitride layer of Mag.
The preferred embodiment of the invention also has, and in described step S4, is sprayed by described the 3rd vaporific nitride layer after covering the second zone of oxidation particle completely, then by rubber, the 3rd nitride layer above the second zone of oxidation particle is polished into smooth plane.
Preferred technical scheme also has, and in described step S5, described sintering range is 80 DEG C.
Embodiment 2
As shown in Figure 1: the present invention is a kind of high-purity coating type polysilicon crucible, comprise crucible body 1, be evenly equipped with several pits 2 on this surface of 1 of described crucible, be attached with the first nitride layer 3, second zone of oxidation 4 and the 3rd nitride layer 5 successively on the described surface being evenly equipped with several pits 2;
Described first nitride layer 3 is by brushing mode, and by the silicon nitride coated of Mag in this 1 the surface of crucible being evenly equipped with several pits 2, the coating thickness scope of described first nitride layer 3 is 6mm;
Described second zone of oxidation 4 is pulverous silicon oxide, and the first nitride layer 3 sprayed pulverous silicon oxide in the Mag not yet condensed by spray regime is surperficial, and described second zone of oxidation 4 forms particulate state on the surface of the first nitride layer 3;
Described 3rd nitride layer 5 is vaporific silicon nitride, and by spraying method by the surface of vaporific silicon nitride spray finishing in the second zone of oxidation 4, until the particle of described second zone of oxidation 4 is capped, described 3rd nitride layer 5 forms shiny surface.
The preferred embodiment of the invention is, described first nitride layer 3 comprises silicon nitride, hydrated barta and caking agent, and described silicon nitride, hydrated barta and caking agent form the first nitride layer 3 by brushing mode after adding deionized water and stirring formation Mag.
The preferred embodiment of the invention also has, and described caking agent is silicic acid.
The preferred embodiment of the invention also has, and the weight ratio of described silicon nitride, hydrated barta, caking agent and deionized water is 100:2:16:10.
The preferred embodiment of the invention also has, and described second zone of oxidation 4 is silicon oxide, and described silicon oxide is reacted by silicon nitride and hyperoxia agent to be made, and described hyperoxia agent is ozone.
Further preferred embodiment of the present invention also has, and the silicon oxide of described second zone of oxidation 4 adopts lance ejection, and the spray speed scope of described spray gun is 8km/h, is 25cm apart from the jet length scope of injected.
The preferred embodiment of the invention also has, and this surface of 1 of described crucible is internal surface and the bead place, upper end of crucible.
Further preferred embodiment of the present invention also has, and the shape of cross section of described pit 2 is Ω shape.
Further preferred embodiment of the present invention also has, and described polysilicon crucible body 1 is a cuboid container, and the length range of described polysilicon crucible upper port is 2.2m, and width range is 0.6m.
Further preferred embodiment of the present invention also has, and the outer side wall of described crucible body 1 is also covered with the first silicon nitride 3.
Based on a brushing method for the coating of above-mentioned high-purity coating type polysilicon crucible, comprise the following steps:
S1, polysilicon crucible body is processed into the surface being evenly equipped with several pits or annular recesses;
S2, be evenly equipped with first nitride layer of brushing Mag on surface of polysilicon crucible body of several pits, and making the first nitride layer be filled in several pits described or annular recesses;
S3, before the first nitride layer condensation of described Mag, in the second zone of oxidation of described first nitride layer surface jet particle shape;
S4 and then spray vaporific the 3rd nitride layer, until the 3rd vaporific nitride layer covers granular second zone of oxidation completely to granular second zone of oxidation surface;
S5, high temperature sintering, until the first nitride layer of Mag, the second zone of oxidation and the 3rd nitride layer condense completely and become an one-piece construction with polysilicon crucible body.
The preferred embodiment of the invention is, in described step S2, described first nitride layer comprises silicon nitride, hydrated barta and caking agent, and described silicon nitride, hydrated barta and caking agent add deionized water and stirring and form Mag.
The preferred embodiment of the invention also has, and in described step S3, described second zone of oxidation is granular silicon oxide, and the granular size scope of described silicon oxide is 4mm
2, described granular silicon oxide adopts lance ejection to the surface of the first nitride layer of Mag.
The preferred embodiment of the invention also has, and in described step S4, is sprayed by described the 3rd vaporific nitride layer after covering the second zone of oxidation particle completely, then by rubber, the 3rd nitride layer above the second zone of oxidation particle is polished into smooth plane.
Preferred technical scheme also has, and in described step S5, described sintering range is 100 DEG C.
Embodiment 3
As shown in Figure 1: the present invention is a kind of high-purity coating type polysilicon crucible, comprise crucible body 1, be evenly equipped with several pits 2 on this surface of 1 of described crucible, be attached with the first nitride layer 3, second zone of oxidation 4 and the 3rd nitride layer 5 successively on the described surface being evenly equipped with several pits 2;
Described first nitride layer 3 is by brushing mode, and by the silicon nitride coated of Mag in this 1 the surface of crucible being evenly equipped with several pits 2, the coating thickness scope of described first nitride layer 3 is 10mm;
Described second zone of oxidation 4 is pulverous silicon oxide, and the first nitride layer sprayed pulverous silicon oxide in the Mag not yet condensed by spray regime is surperficial, and described second zone of oxidation 4 forms particulate state on the surface of the first nitride layer 3;
Described 3rd nitride layer 5 is vaporific silicon nitride, by spraying method by the surface of vaporific silicon nitride spray finishing in the second zone of oxidation 4, until the particle of described second zone of oxidation 4 is capped, and described 3rd nitride layer 5 shiny surface.
The preferred embodiment of the invention is, described first nitride layer 3 comprises silicon nitride, hydrated barta and caking agent, and described silicon nitride, hydrated barta and caking agent form the first nitride layer 3 by brushing mode after adding deionized water and stirring formation Mag.
The preferred embodiment of the invention also has, and described caking agent is polyvalent alcohol.
The preferred embodiment of the invention also has, and the weight ratio of described silicon nitride, hydrated barta, caking agent and deionized water is 100:3:17:12.
The preferred embodiment of the invention also has, and described second zone of oxidation 4 is silicon oxide, and described silicon oxide is reacted by silicon nitride and hyperoxia agent to be made, and described hyperoxia agent is the vitriol oil.
Further preferred embodiment of the present invention also has, and the silicon oxide of described second zone of oxidation 4 adopts lance ejection, and the spray speed scope of described spray gun is 11km/h, is 30cm apart from the jet length scope of injected.
The preferred embodiment of the invention also has, and this surface of 1 of described crucible is internal surface and the bead place, upper end of crucible.
Further preferred embodiment of the present invention also has, and the shape of cross section of described pit 2 is Ω shape.
Further preferred embodiment of the present invention also has, and described polysilicon crucible body 1 is a cuboid container, and the length range of described polysilicon crucible upper port is 2.4m, and width range is 0.7m.
Further preferred embodiment of the present invention also has, and the outer side wall of described crucible body 1 is also covered with the first silicon nitride layer 3.
Based on a brushing method for the coating of above-mentioned high-purity coating type polysilicon crucible, comprise the following steps:
S1, polysilicon crucible body is processed into the surface being evenly equipped with several pits or annular recesses;
S2, be evenly equipped with first nitride layer of brushing Mag on surface of polysilicon crucible body of several pits, and making the first nitride layer be filled in several pits described or annular recesses;
S3, before the first nitride layer condensation of described Mag, in the second zone of oxidation of described first nitride layer surface jet particle shape;
S4 and then spray vaporific the 3rd nitride layer, until the 3rd vaporific nitride layer covers granular second zone of oxidation completely to granular second zone of oxidation surface;
S5, high temperature sintering, until the first nitride layer of Mag, the second zone of oxidation and the 3rd nitride layer condense completely and become an one-piece construction with polysilicon crucible body.
The preferred embodiment of the invention is, in described step S2, described first nitride layer comprises silicon nitride, hydrated barta and caking agent, and described silicon nitride, hydrated barta and caking agent add deionized water and stirring and form Mag.
The preferred embodiment of the invention also has, and in described step S3, described second zone of oxidation is granular silicon oxide, and the granular size scope of described silicon oxide is 6mm
2, described granular silicon oxide adopts lance ejection to the surface of the first nitride layer of Mag.
The preferred embodiment of the invention also has, and in described step S4, is sprayed by described the 3rd vaporific nitride layer after covering the second zone of oxidation particle completely, then by rubber, the 3rd nitride layer above the second zone of oxidation particle is polished into smooth plane.
Preferred technical scheme also has, and in described step S5, described sintering range is 120 DEG C.
Embodiment 4
As shown in Figure 1: the present invention is a kind of high-purity coating type polysilicon crucible, comprise crucible body 1, be evenly equipped with several annular recessess on this surface of 1 of described crucible, be attached with the first nitride layer 3, second zone of oxidation 4 and the 3rd nitride layer 5 successively on the described surface being evenly equipped with several annular recessess;
Described first nitride layer 3 is by brushing mode, and by the silicon nitride coated of Mag in the crucible surface being originally evenly equipped with several annular recessess, the coating thickness scope of described first nitride layer 3 is 15mm;
Described second zone of oxidation 4 is pulverous silicon oxide, and the first nitride layer 3 sprayed pulverous silicon oxide in the Mag not yet condensed by spray regime is surperficial, and described second zone of oxidation 4 forms particulate state on the surface of the first nitride layer 3;
Described 3rd nitride layer 5 is vaporific silicon nitride, and by spraying method by the surface of vaporific silicon nitride spray finishing in the second zone of oxidation 4, until the particle of described second zone of oxidation 4 is capped, described 3rd nitride layer 5 forms shiny surface.
The preferred embodiment of the invention is, described first nitride layer 3 comprises silicon nitride, hydrated barta and caking agent, and described silicon nitride, hydrated barta and caking agent form the first nitride layer 3 by brushing mode after adding deionized water and stirring formation Mag.
The preferred embodiment of the invention also has, and described caking agent is organic polyethylene alcohol.
The preferred embodiment of the invention also has, and the weight ratio of described silicon nitride, hydrated barta, caking agent and deionized water is 100:4:18:13.
The preferred embodiment of the invention also has, and described second zone of oxidation 4 is silicon oxide, and described silicon oxide is reacted by silicon nitride and hyperoxia agent to be made, and described hyperoxia agent is nitric acid.
Further preferred embodiment of the present invention also has, and the silicon oxide of described second zone of oxidation 4 adopts lance ejection, and the spray speed scope of described spray gun is 15km/h, is 40cm apart from the jet length scope of injected.
The preferred embodiment of the invention also has, and this surface of 1 of described crucible is internal surface and the bead place, upper end of crucible.
Further preferred embodiment of the present invention also has, and the shape of cross section of described annular recesses is dove-tail.
Further preferred embodiment of the present invention also has, and described polysilicon crucible body 1 is a cuboid container, and the length range of described polysilicon crucible upper port is 2.8m, and width range is 0.8m.
Further preferred embodiment of the present invention also has, and the outer side wall of described crucible body 1 is also covered with the first silicon nitride layer 3.
Based on a brushing method for the coating of above-mentioned high-purity coating type polysilicon crucible, comprise the following steps:
S1, polysilicon crucible body is processed into the surface being evenly equipped with several pits or annular recesses;
S2, be evenly equipped with first nitride layer of brushing Mag on surface of polysilicon crucible body of several pits, and making the first nitride layer be filled in several pits described or annular recesses;
S3, before the first nitride layer condensation of described Mag, in the second zone of oxidation of described first nitride layer surface jet particle shape;
S4 and then spray vaporific the 3rd nitride layer, until the 3rd vaporific nitride layer covers granular second zone of oxidation completely to granular second zone of oxidation surface;
S5, high temperature sintering, until the first nitride layer of Mag, the second zone of oxidation and the 3rd nitride layer condense completely and become an one-piece construction with polysilicon crucible body.
The preferred embodiment of the invention is, in described step S2, described first nitride layer comprises silicon nitride, hydrated barta and caking agent, and described silicon nitride, hydrated barta and caking agent add deionized water and stirring and form Mag.
The preferred embodiment of the invention also has, and in described step S3, described second zone of oxidation is granular silicon oxide, and the granular size scope of described silicon oxide is 8mm
2, described granular silicon oxide adopts lance ejection to the surface of the first nitride layer of Mag.
The preferred embodiment of the invention also has, and in described step S4, is sprayed by described the 3rd vaporific nitride layer after covering the second zone of oxidation particle completely, then by rubber, the 3rd nitride layer above the second zone of oxidation particle is polished into smooth plane.
Preferred technical scheme also has, and in described step S5, described sintering range is 150 DEG C.
Embodiment 5
As shown in Figure 1: the present invention is a kind of high-purity coating type polysilicon crucible, comprise crucible body 1, be evenly equipped with annular recesses on this surface of 1 of described crucible, be attached with the first nitride layer 3, second zone of oxidation and 4 the 3rd nitride layers 5 on the described surface being evenly equipped with several annular recessess successively;
Described first nitride layer is by brushing mode, and by the silicon nitride coated of Mag in this 1 the surface of crucible being evenly equipped with several annular recessess, the coating thickness scope of described first nitride layer 3 is 19mm;
Described second zone of oxidation 4 is pulverous silicon oxide, and the first nitride layer sprayed pulverous silicon oxide in the Mag not yet condensed by spray regime is surperficial, and described second zone of oxidation 4 forms particulate state on the surface of the first nitride layer 3;
Described 3rd nitride layer 5 is vaporific silicon nitride, by spraying method, vaporific silicon nitride spray finishing is surperficial in the second zone of oxidation 4, until the particle of described second zone of oxidation 4 is capped, described 3rd nitride layer 5 forms shiny surface.
The preferred embodiment of the invention is, described first nitride layer 3 comprises silicon nitride, hydrated barta and caking agent, and described silicon nitride, hydrated barta and caking agent form the first nitride layer 3 by brushing mode after adding deionized water and stirring formation Mag.
The preferred embodiment of the invention also has, and described caking agent is for there being acrylate.
The preferred embodiment of the invention also has, and the weight ratio of described silicon nitride, hydrated barta, caking agent and deionized water is 100:5:25:14.
The preferred embodiment of the invention also has, and described second zone of oxidation 4 is silicon oxide, and described silicon oxide is reacted by silicon nitride and hyperoxia agent to be made, and described hyperoxia agent is potassiumchromate.
Further preferred embodiment of the present invention also has, and the silicon oxide of described second zone of oxidation 4 adopts lance ejection, and the spray speed scope of described spray gun is 18km/h, is 80cm apart from the jet length scope of injected.
The preferred embodiment of the invention also has, and this surface of 1 of described crucible is internal surface and the bead place, upper end of crucible.
Further preferred embodiment of the present invention also has, and the shape of cross section of described annular recesses is dove-tail.
Further preferred embodiment of the present invention also has, and described polysilicon crucible body 1 is a cuboid container, and the length range of described polysilicon crucible upper port is 2.8m, and width range is 0.9m.
The further preferred described scheme of the present invention also has, and the outer side wall of described crucible body 1 is also covered with the first silicon nitride layer 3.
Based on a brushing method for the coating of above-mentioned high-purity coating type polysilicon crucible, comprise the following steps:
S1, polysilicon crucible body is processed into the surface being evenly equipped with several pits or annular recesses;
S2, be evenly equipped with first nitride layer of brushing Mag on surface of polysilicon crucible body of several pits, and making the first nitride layer be filled in several pits described or annular recesses;
S3, before the first nitride layer condensation of described Mag, in the second zone of oxidation of described first nitride layer surface jet particle shape;
S4 and then spray vaporific the 3rd nitride layer, until the 3rd vaporific nitride layer covers granular second zone of oxidation completely to granular second zone of oxidation surface;
S5, high temperature sintering, until the first nitride layer of Mag, the second zone of oxidation and the 3rd nitride layer condense completely and become an one-piece construction with polysilicon crucible body.
The preferred embodiment of the invention is, in described step S2, described first nitride layer comprises silicon nitride, hydrated barta and caking agent, and described silicon nitride, hydrated barta and caking agent add deionized water and stirring and form Mag.
The preferred embodiment of the invention also has, and in described step S3, described second zone of oxidation is granular silicon oxide, and the granular size scope of described silicon oxide is 10mm
2, described granular silicon oxide adopts lance ejection to the surface of the first nitride layer of Mag.
The preferred embodiment of the invention also has, and in described step S4, is sprayed by described the 3rd vaporific nitride layer after covering the second zone of oxidation particle completely, then by rubber, the 3rd nitride layer above the second zone of oxidation particle is polished into smooth plane.
Preferred technical scheme also has, and in described step S5, described sintering range is 180 DEG C.
Embodiment 6
As shown in Figure 1: the present invention is a kind of high-purity coating type polysilicon crucible, comprise crucible body 1, be evenly equipped with several annular recessess on this surface of 1 of described crucible, be attached with the first nitride layer 3, second zone of oxidation 4 and the 3rd nitride layer 5 successively on the described surface being evenly equipped with several annular recessess;
Described first nitride layer 3 is by brushing mode, and by the silicon nitride coated of Mag in the crucible surface being originally evenly equipped with several annular recessess, the coating thickness scope of described first nitride layer 3 is 20mm;
Described second zone of oxidation 4 is pulverous silicon oxide, and the first nitride layer 3 sprayed pulverous silicon oxide in the Mag not yet condensed by spray regime is surperficial, and described second zone of oxidation 4 forms particulate state on the surface of the first nitride layer 3;
Described 3rd nitride layer 5 is vaporific silicon nitride, and by spraying method by the surface of vaporific silicon nitride spray finishing in the second zone of oxidation 4, until the particle of described second zone of oxidation 4 is capped, described 3rd nitride layer 5 forms shiny surface.
The preferred embodiment of the invention is, described first nitride layer 3 comprises silicon nitride, hydrated barta and caking agent, and described silicon nitride, hydrated barta and caking agent form the first nitrogenize 3 by brushing mode after adding deionized water and stirring formation Mag.
The preferred embodiment of the invention also has, and described caking agent is acrylate.
The preferred embodiment of the invention also has, and the weight ratio of described silicon nitride, hydrated barta, caking agent and deionized water is 100:5:30:15.
The preferred embodiment of the invention also has, and described second zone of oxidation 4 is silicon oxide, and described silicon oxide is reacted by silicon nitride and hyperoxia agent to be made, and described hyperoxia agent is potassium permanganate.
Further preferred embodiment of the present invention also has, and the silicon oxide of described second zone of oxidation 4 adopts lance ejection, and the spray speed scope of described spray gun is 20km/h, is 100cm apart from the jet length scope of injected.
The preferred embodiment of the invention also has, and this surface of 1 of described crucible is internal surface and the bead place, upper end of crucible.
Further preferred embodiment of the present invention also has, and the shape of cross section of described annular recesses is dove-tail.
Further preferred embodiment of the present invention also has, and described polysilicon crucible body 1 is a cuboid container, and the length range of described polysilicon crucible upper port is 3m, and width range is 1m.
Further preferred embodiment of the present invention also has, and the outer side wall of described crucible body 1 is also covered with the first silicon nitride layer 3.
Based on a brushing method for the coating of above-mentioned high-purity coating type polysilicon crucible, comprise the following steps:
S1, polysilicon crucible body is processed into the surface being evenly equipped with several pits or annular recesses;
S2, be evenly equipped with first nitride layer of brushing Mag on surface of polysilicon crucible body of several pits, and making the first nitride layer be filled in several pits described or annular recesses;
S3, before the first nitride layer condensation of described Mag, in the second zone of oxidation of described first nitride layer surface jet particle shape;
S4 and then spray vaporific the 3rd nitride layer, until the 3rd vaporific nitride layer covers granular second zone of oxidation completely to granular second zone of oxidation surface;
S5, high temperature sintering, until the first nitride layer of Mag, the second zone of oxidation and the 3rd nitride layer condense completely and become an one-piece construction with polysilicon crucible body.
The preferred embodiment of the invention is, in described step S2, described first nitride layer comprises silicon nitride, hydrated barta and caking agent, and described silicon nitride, hydrated barta and caking agent add deionized water and stirring and form Mag.
The preferred embodiment of the invention also has, and in described step S3, described second zone of oxidation is granular silicon oxide, and the granular size scope of described silicon oxide is 10mm
2, described granular silicon oxide adopts lance ejection to the surface of the first nitride layer of Mag.
The preferred embodiment of the invention also has, and in described step S4, is sprayed by described the 3rd vaporific nitride layer after covering the second zone of oxidation particle completely, then by rubber, the 3rd nitride layer above the second zone of oxidation particle is polished into smooth plane.
Preferred technical scheme also has, and in described step S5, described sintering range is 200 DEG C.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing from the technology of the present invention principle; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. a high-purity coating type polysilicon crucible, comprise crucible body (1), it is characterized in that, several pits or annular recesses (2) is evenly equipped with on the surface of described crucible this (1), the first nitride layer (3), the second zone of oxidation (4) and the 3rd nitride layer (5) is attached with successively on the described surface being evenly equipped with several pits or annular recesses, the surface of described crucible this (1) is internal surface and the bead place, upper end of crucible, and the shape of cross section of described pit is the shape of cross section of Ω ring connected in star is dove-tail;
Described first nitride layer (3) is by brushing mode, by the silicon nitride coated of Mag in this surface of (1) of crucible being evenly equipped with several pits or annular recesses (2), the coating thickness scope of described first nitride layer (3) is 2 ~ 20mm;
Described second zone of oxidation (3) is pulverous silicon oxide, the first nitride layer (3) sprayed pulverous silicon oxide in the Mag not yet condensed by spray regime is surperficial, and described second zone of oxidation (4) forms particulate state on the surface of the first nitride layer (2);
Described 3rd nitride layer (5) is vaporific silicon nitride, by spraying method by the surface of vaporific silicon nitride spray finishing in the second zone of oxidation (4), until the particle of described second zone of oxidation (4) is capped, described 3rd nitride layer (5) forms shiny surface.
2. high-purity coating type polysilicon crucible as claimed in claim 1, it is characterized in that, described first nitride layer (3) comprises silicon nitride, hydrated barta and caking agent, described silicon nitride, hydrated barta and caking agent form the first nitride layer (2) by brushing mode after adding deionized water and stirring formation Mag, the silicon oxide of described second zone of oxidation (4) adopts lance ejection, the spray speed scope of described spray gun is 5 ~ 20km/h, is 20 ~ 100cm apart from the jet length scope of injected.
3. high-purity coating type polysilicon crucible as claimed in claim 2, is characterized in that, described caking agent is the one in organosilane, silicic acid, polyvalent alcohol, polyvinyl alcohol and acrylate.
4. high-purity coating type polysilicon crucible as claimed in claim 2, is characterized in that, the weight ratio of described silicon nitride, hydrated barta, caking agent and deionized water is 100:5 ~ 1:15 ~ 30:8 ~ 15.
5. high-purity coating type polysilicon crucible as claimed in claim 1, it is characterized in that, described second zone of oxidation (4) is silicon oxide, described silicon oxide is reacted by silicon nitride and hyperoxia agent to be made, and described hyperoxia agent is any one in hydrogen peroxide, ozone, the vitriol oil, nitric acid, potassiumchromate, potassium permanganate.
6., based on a brushing method for the coating of high-purity coating type polysilicon crucible described in any one in claim 1-5, it is characterized in that, comprise the following steps:
S1, polysilicon crucible body (1) is processed into the surface being evenly equipped with several pits or annular recesses (2);
S2, be evenly equipped with first nitride layer (3) of brushing Mag on surface of polysilicon crucible body (1) of several pits (2) or annular recesses, and making the first nitride layer (3) be filled in several pits described or annular recesses (2);
S3, described Mag the first nitride layer (3) condensation before, in second zone of oxidation (4) of the surperficial jet particle shape of described first nitride layer (3);
S4 and then spray the 3rd vaporific nitride layer (5), until the 3rd vaporific nitride layer (5) covers granular second zone of oxidation (4) completely to granular second zone of oxidation (4) surface;
S5, high temperature sintering, until first nitride layer (3) of Mag, the second zone of oxidation (4) and the 3rd nitride layer (5) condense completely and become an one-piece construction with polysilicon crucible body (1).
7. the brushing method of coating as claimed in claim 6, it is characterized in that, in described step S2, described first nitride layer (3) comprises silicon nitride, hydrated barta and caking agent, and described silicon nitride, hydrated barta and caking agent add deionized water and stirring and form Mag.
8. the brushing method of coating as claimed in claim 6, it is characterized in that, in described step S3, described second zone of oxidation (4) is granular silicon oxide, and the granular size scope of described silicon oxide is 2 ~ 10mm
2, described granular silicon oxide adopts lance ejection to the surface of first nitride layer (3) of Mag.
9. the brushing method of coating as claimed in claim 6, it is characterized in that, in described step S4, described the 3rd vaporific nitride layer (5) is sprayed after covering the second zone of oxidation (4) particle completely, then by rubber, the 3rd nitride layer (5) above the second zone of oxidation (4) particle is polished into smooth plane.
10. as the brushing method of the coating in claim 6 to 9 as described in any one, it is characterized in that, in described step S5, described sintering range is 80 ~ 200 DEG C.
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