CN105154971B - A kind of high-purity coating type polysilicon crucible and the brushing method of coating thereof - Google Patents
A kind of high-purity coating type polysilicon crucible and the brushing method of coating thereof Download PDFInfo
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Abstract
The present invention relates to a kind of high-purity coating type polysilicon crucible and the brushing method of coating thereof, including crucible body, be evenly equipped with several pits or annular groove on the surface of crucible body, be attached with the first nitration case, the second oxide layer and the 3rd nitration case on surface successively；First nitration case of breast paddle is brushed on the surface of crucible body, the silicon oxide of the second oxide layer powder is ejected in the surface of breast oar, pass through spraying method again by vaporific silicon nitride spray finishing in the surface of the second oxide layer, until the granule of the second oxide layer is capped, the 3rd nitration case forms shiny surface.It is strong that the brushing method of described high-purity coating type polysilicon crucible and coating thereof has coating covering power, and stability is high, has high-isolation, prevents crucible body from participating in the feature of reaction in preparing polysilicon process.
Description
Technical field
The present invention relates to manufacture of solar cells equipment technical field, be specifically related to a kind of high-purity coating type polysilicon crucible and the brushing method of coating thereof.
Background technology
It is known that world today's supply of electric power is the most nervous, the utilization of photovoltaic technology can alleviate this situation effectively.Photovoltaic generation mainly has 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, consuming the same energy, polycrystalline output will be 6～7 times of monocrystalline, thus polycrystalline finds broad application in recent years.
In recent years, increasingly mature along with solar energy generation technology, solaode obtains extensive application at numerous areas such as industry, agricultural and space flight.At present, according to the difference of material therefor, solaode can be divided into: silicon solar cell, compound film solaode and polymer multi-layer modified electrode solaode, 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 solaode preparation process is relatively simple, has the advantages such as cost low energy is low, and therefore polysilicon solar cell application is relatively broad.
Crucible is the required equipment that polycrystalline silicon ingot casting produces.At present, production of polysilicon mainly uses silica crucible, this is because silica source enriches, purity is high, and cheap.Although using silica crucible to produce polycrystalline silicon ingot casting contribute to reducing production cost, but it having a drawback in that the problem that silicon ingot is the most cracking when cooling.This is primarily due to: the silicon dioxde reaction that melted silicon can be in contact with it, and forms silicon monoxide and oxygen；Wherein, oxygen can pollute silicon, and silicon monoxide has volatility；And it also can form carborundum and carbon monoxide with the graphite member in stove, the carbon monoxide generated then can be with melted pasc reaction, forming volatile silicon monoxide, carborundum, metallic traces or the carbide of adulterant, oxide and carbon, carbon can pollute silicon.Above-mentioned reaction between silicon dioxide and molten silicon promotes silicon to be attached on crucible.But owing to the thermal coefficient of expansion between silicon dioxide and silicon both materials is different, cause silicon ingot easily to ftracture when cooling.
In order to avoid silicon ingot ftractures when cooling, it usually needs use protective coating at inner surface of crucible, silicon dioxide and molten silicon thus can be stoped to react, and then reduce silicon ingot pollution and cracking.This coating must be sufficiently thick to stop silicon dioxide to react with molten silicon, and must assure that the high-purity of this coating is to prevent its interior objectionable impurities from polluting silicon.
Prior art has employing chemical vapour deposition technique to prepare silicon nitride coating, such as disclose a kind of crucible silicon nitride coating being deposited at 1250 DEG C preparation by chemical gaseous phase in the United States Patent (USP) of the patent No. 4741925.And for example the PCT Publication of Patent No. WO2004053207A1 is by plasma spraying silicon nitride coating.Although said method is prevented from the problem that silicon nitride coating peels or flakes off, but costly and operation is complicated for the method equipment needed thereby price.
In order to cost-effective, prior art mainly uses silicon nitride as crucible coating layer.Solar energy industry uses the most universal method mainly to be aoxidized under controlled burnout cycle under the high temperature of 700～1450 DEG C by silicon nitride coating at present, so that producing bonding between silicon nitride particle and between silicon nitride particle and silica crucible.The defect of the method is that silicon nitride coating dust in thermal spray process is big, and local location tends to have bubble, and calcining heat is higher, and energy consumption is big.
The crucible additionally used currently for polysilicon fusion-crystallization, the most all uses high purity graphite material to make, and self manufacturing cost is bigger；And the polycrystalline silicon ingot casting that graphite crucible crystallizes out, its impurity content is higher, and effective recovery rate of silicon ingot is the lowest, and there is the defects such as using effect is undesirable, with fashion can not large-scale production and application, therefore, polysilicon crucible has wide market prospect.
In prior art, it will usually at one layer of silicon nitride coating of surface-coated of crucible.But the silicon nitride material of densification must enclose and liquid-phase sintering under hot environment at nitrogen protective atmosphere; and size shrinks more than 10% than before sintering after the finest and close silicon nitride material sintering; so the silicon nitride layer of quartz crucible surface coating is extremely difficult to high fine and close degree, it is impossible to meet production requirement.
Summary of the invention
It is an object of the invention to overcome defect of the prior art, design a kind of high-purity coating type polysilicon crucible so that it is have coating covering power strong, stability is high, has high-isolation, prevents crucible body from participating in the feature of reaction in preparing polysilicon process.
For achieving the above object, the technical solution adopted in the present invention is:
A kind of high-purity coating type polysilicon crucible, including crucible body, it is evenly equipped with several pits or annular groove on described crucible surface originally, the first nitration case, the second oxide layer and the 3rd nitration case it is attached with successively on the described surface being evenly equipped with several pits or annular groove, the surface of described crucible body is at the inner surface of crucible and upper end bead, the shape of cross section of described pit be the shape of cross section of Ω ring connected in star be dove-tail；
Described first nitration case is by brushing mode, and by the silicon nitride coated of Mag in the surface of the crucible body being evenly equipped with several pits or annular groove, the coating thickness scope of described first nitration case is 2 ~ 20
mm；
Described second oxide layer is the silicon oxide of powder, by spray regime, the silicon oxide of powder is sprayed the first nitration case surface in the Mag not yet condensed, and described second oxide layer forms graininess on the surface of the first nitration case；
Described 3rd nitration case is vaporific silicon nitride, and by spraying method by vaporific silicon nitride spray finishing in the surface of the second oxide layer, until the granule of described second oxide layer is capped, described 3rd nitration case forms shiny surface.
Wherein preferably technical scheme is, described first nitration case includes silicon nitride, barium hydroxide and bonding agent, described silicon nitride, barium hydroxide and bonding agent form the first nitration case by brushing mode after adding deionized water stirring formation Mag, the silicon oxide of described second oxide layer uses lance ejection, the spray speed scope of described spray gun is 5 ~ 20km/h, and the jet length scope away from injected is 20 ~ 100 cm.
Preferably technical scheme also has, and described bonding agent is the one in organosilan, silicic acid, polyhydric alcohol, polyvinyl alcohol and acrylate.
Preferably technical scheme also has, and the weight ratio of described silicon nitride, barium hydroxide, bonding agent and deionized water is 100:5 ~ 1:15 ~ 30:8 ~ 15.
Preferably technical scheme also has, and described second oxide layer is silicon oxide, and described silicon oxide is reacted with hyperoxia agent by silicon nitride to be made, and described hyperoxia agent is any one in hydrogen peroxide, ozone, concentrated sulphuric acid, nitric acid, Neutral potassium chromate, potassium permanganate.
Further preferred technical scheme also has, and described polysilicon crucible body is a cuboid container, and the length range of described polysilicon crucible upper port is 2 ~ 3 m, and width range is 0.5 ~ 1 m.
Further preferred technical scheme also has, and is also covered with the first silicon nitride layer on the lateral wall of described crucible body.
Further object is that, designing the brushing method of the coating of a kind of high-purity coating type polysilicon crucible so that it is it is strong that the coating after brushing has coating covering power, stability is high, there is high-isolation, prevent crucible body from participating in the feature of reaction in preparing polysilicon process.
For achieving the above object, another technical scheme of the present invention is:
The brushing method of a kind of coating based on above-mentioned high-purity coating type polysilicon crucible, comprises the following steps:
S1, polysilicon crucible body is processed into the surface being evenly equipped with several pits or annular groove；
S2, the first nitration case of brushing Mag on the surface of the polysilicon crucible body being evenly equipped with several pits or annular groove, and make the first nitration case be filled in several pits described or annular groove；
S3, described Mag first nitration case condense before, described first nitration case surface spray granular second oxide layer；
S4, the most again to granular second vaporific the 3rd nitration case of oxide layer surface injection, until the 3rd vaporific nitration case is completely covered granular second oxide layer；
S5, high temperature sintering, until the first nitration case of Mag, the second oxide layer and the 3rd nitration case condense completely and become an overall structure with polysilicon crucible body.
Wherein preferably technical scheme is, in described step S2, described first nitration case includes that silicon nitride, barium hydroxide and bonding agent, described silicon nitride, barium hydroxide and bonding agent add deionized water stirring and form Mag.
Preferably technical scheme also has, and in described step S3, described second oxide layer is granular silicon oxide, and the granular size scope of described silicon oxide is 2 ~ 10mm2, described granular silicon oxide uses lance ejection to the surface of the first nitration case of Mag.
Preferably technical scheme also has, and in described step S4, after described the 3rd vaporific nitration case injection is completely covered the second oxide layer granule, then by rubber, the 3rd nitration case above the second oxide layer granule is polished into smooth plane.
Preferably technical scheme also has, and in described step S5, described sintering range is 80 ~ 200 DEG C.
The advantage of high-purity coating type polysilicon crucible of the present invention and having the beneficial effects that: preparation cost is low and coating covering power is strong, effectively preventing the sintering shrinkage of silicon nitride, stability is high, has high-isolation, prevent crucible body from participating in reaction in preparing polysilicon process, meet production requirement.
In the first nitration case of described high-purity coating type polysilicon crucible, the binding agent used is organosilan, silicic acid, polyhydric alcohol, polyvinyl alcohol or the acrylate that sticking temperature is relatively low, on the one hand above-mentioned binding agent can reduce the temperature of subsequent calcination, calcining heat is reduced to 80 DEG C～200 DEG C, thus reduces energy consumption；On the other hand improve slurry viscosity, reduce the Dust Capacity produced in follow-up spraying process, it is ensured that the health of operator, reduce environmental pollution；Additionally, it can also improve the adhesion strength of silicon nitride coating and crucible, improve the mechanical property of coating.Further, the consumption of binding agent and silicon nitride is also controlled by the present invention.
In the first nitration case, add barium hydroxide, react with silicon and boron impurities therein under high temperature, generate BOH gas, volatilize with SiO, such that it is able to play the effect except boron.
Further, since be evenly equipped with several pits or annular groove on this surface of crucible, and the shape of cross section of described pit be the shape of cross section of Ω ring connected in star be dove-tail.The throat structure that namely inner chamber is less compared with large port, thus can improve the adhesive strength of the first nitration case and this surface of crucible further.
Accompanying drawing explanation
Fig. 1 is the partial structurtes schematic diagram of the present invention high-purity coating type polysilicon crucible.
In figure: 1, crucible body；2, pit；3, the first nitration case；4, the second oxide layer；5, the 3rd nitration case.
Detailed description of the invention
Below in conjunction with the accompanying drawings and embodiment, the detailed description of the invention of the present invention is further described.Following example are only used for clearly illustrating technical scheme, 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, including crucible body 1, it is evenly equipped with several pits 2 on the surface of described crucible body 1, is attached with the first nitration case the 3, second oxide layer 4 and the 3rd nitration case 5 on the described surface being evenly equipped with several pits 2 successively；
Described first nitration case 3 is by brushing mode, and by the silicon nitride coated of Mag in the surface of the crucible body 1 being evenly equipped with several pits 2, the coating thickness scope of described first nitration case 3 is 2 mm；
Described second oxide layer 4 is the silicon oxide of powder, by spray regime, the silicon oxide of powder is sprayed the first nitration case 3 surface in the Mag not yet condensed, and described second oxide layer 4 forms graininess on the surface of the first nitration case 3；
Described 3rd nitration case 5 is vaporific silicon nitride, and by spraying method by vaporific silicon nitride spray finishing in the surface of the second oxide layer 4, until the granule of described second oxide layer 4 is capped, described 3rd nitration case 5 forms shiny surface.
Currently preferred technical scheme is, described first nitration case 3 includes that silicon nitride, barium hydroxide and bonding agent, described silicon nitride, barium hydroxide and bonding agent add after deionized water stirring forms Mag and forms the first nitration case 3 by brushing mode.
The preferred embodiment of the invention also has, and described bonding agent is organosilan.
The preferred embodiment of the invention also has, and the weight ratio of described silicon nitride, barium hydroxide, bonding agent and deionized water is 100:1:15:8.
The preferred embodiment of the invention also has, and described second oxide layer 4 is silicon oxide, and described silicon oxide is reacted with hyperoxia agent by silicon nitride 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 2nd 4 uses lance ejection, and the spray speed scope of described spray gun is 5km/h, and the jet length scope away from injected is 20cm.
The preferred embodiment of the invention also has, at the inner surface that surface is crucible of described crucible body 1 and upper end bead.
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 is also covered with the first silicon nitride layer 3 on the lateral wall of described crucible body 1.
The brushing method of a kind of coating based on above-mentioned high-purity coating type polysilicon crucible, comprises the following steps:
S1, polysilicon crucible body is processed into the surface being evenly equipped with several pits or annular groove；
S2, the first nitration case of brushing Mag on the surface of the polysilicon crucible body being evenly equipped with several pits, and make the first nitration case be filled in several pits described or annular groove；
S3, described Mag first nitration case condense before, described first nitration case surface spray granular second oxide layer；
S4, the most again to granular second vaporific the 3rd nitration case of oxide layer surface injection, until the 3rd vaporific nitration case is completely covered granular second oxide layer；
S5, high temperature sintering, until the first nitration case of Mag, the second oxide layer and the 3rd nitration case condense completely and become an overall structure with polysilicon crucible body.
The preferred embodiment of the invention is, in described step S2, described first nitration case includes that silicon nitride, barium hydroxide and bonding agent, described silicon nitride, barium hydroxide and bonding agent add deionized water stirring and form Mag.
The preferred embodiment of the invention also has, and in described step S3, described second oxide layer is granular silicon oxide, and the granular size scope of described silicon oxide is 2mm2, described granular silicon oxide uses lance ejection to the surface of the first nitration case of Mag.
The preferred embodiment of the invention also has, and in described step S4, after described the 3rd vaporific nitration case injection is completely covered the second oxide layer granule, then by rubber, the 3rd nitration case above the second oxide layer granule is polished into smooth plane.
Preferably 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, including crucible body 1, it is evenly equipped with several pits 2 on the surface of described crucible body 1, is attached with the first nitration case the 3, second oxide layer 4 and the 3rd nitration case 5 on the described surface being evenly equipped with several pits 2 successively；
Described first nitration case 3 is by brushing mode, and by the silicon nitride coated of Mag in the surface of the crucible body 1 being evenly equipped with several pits 2, the coating thickness scope of described first nitration case 3 is 6mm；
Described second oxide layer 4 is the silicon oxide of powder, by spray regime, the silicon oxide of powder is sprayed the first nitration case 3 surface in the Mag not yet condensed, and described second oxide layer 4 forms graininess on the surface of the first nitration case 3；
Described 3rd nitration case 5 is vaporific silicon nitride, and by spraying method by vaporific silicon nitride spray finishing in the surface of the second oxide layer 4, until the granule of described second oxide layer 4 is capped, described 3rd nitration case 5 forms shiny surface.
The preferred embodiment of the invention is, described first nitration case 3 includes that silicon nitride, barium hydroxide and bonding agent, described silicon nitride, barium hydroxide and bonding agent add after deionized water stirring forms Mag and forms the first nitration case 3 by brushing mode.
The preferred embodiment of the invention also has, and described bonding agent is silicic acid.
The preferred embodiment of the invention also has, and the weight ratio of described silicon nitride, barium hydroxide, bonding agent and deionized water is 100:2:16:10.
The preferred embodiment of the invention also has, and described second oxide layer 4 is silicon oxide, and described silicon oxide is reacted with hyperoxia agent by silicon nitride 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 oxide layer 4 uses lance ejection, and the spray speed scope of described spray gun is 8km/h, and the jet length scope away from injected is 25 cm.
The preferred embodiment of the invention also has, at the inner surface that surface is crucible of described crucible body 1 and upper end bead.
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 0.6 m.
Further preferred embodiment of the present invention also has, and is also covered with the first silicon nitride 3 on the lateral wall of described crucible body 1.
The brushing method of a kind of coating based on above-mentioned high-purity coating type polysilicon crucible, comprises the following steps:
S1, polysilicon crucible body is processed into the surface being evenly equipped with several pits or annular groove；
S2, the first nitration case of brushing Mag on the surface of the polysilicon crucible body being evenly equipped with several pits, and make the first nitration case be filled in several pits described or annular groove；
S3, described Mag first nitration case condense before, described first nitration case surface spray granular second oxide layer；
S4, the most again to granular second vaporific the 3rd nitration case of oxide layer surface injection, until the 3rd vaporific nitration case is completely covered granular second oxide layer；
S5, high temperature sintering, until the first nitration case of Mag, the second oxide layer and the 3rd nitration case condense completely and become an overall structure with polysilicon crucible body.
The preferred embodiment of the invention is, in described step S2, described first nitration case includes that silicon nitride, barium hydroxide and bonding agent, described silicon nitride, barium hydroxide and bonding agent add deionized water stirring and form Mag.
The preferred embodiment of the invention also has, and in described step S3, described second oxide layer is granular silicon oxide, and the granular size scope of described silicon oxide is 4mm2, described granular silicon oxide uses lance ejection to the surface of the first nitration case of Mag.
The preferred embodiment of the invention also has, and in described step S4, after described the 3rd vaporific nitration case injection is completely covered the second oxide layer granule, then by rubber, the 3rd nitration case above the second oxide layer granule is polished into smooth plane.
Preferably 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, including crucible body 1, it is evenly equipped with several pits 2 on the surface of described crucible body 1, is attached with the first nitration case the 3, second oxide layer 4 and the 3rd nitration case 5 on the described surface being evenly equipped with several pits 2 successively；
Described first nitration case 3 is by brushing mode, and by the silicon nitride coated of Mag in the surface of the crucible body 1 being evenly equipped with several pits 2, the coating thickness scope of described first nitration case 3 is 10 mm；
Described second oxide layer 4 is the silicon oxide of powder, by spray regime, the silicon oxide of powder is sprayed the first nitration case surface in the Mag not yet condensed, and described second oxide layer 4 forms graininess on the surface of the first nitration case 3；
Described 3rd nitration case 5 is vaporific silicon nitride, by spraying method by vaporific silicon nitride spray finishing in the surface of the second oxide layer 4, until the granule of described second oxide layer 4 is capped, and described 3rd nitration case 5 shiny surface.
The preferred embodiment of the invention is, described first nitration case 3 includes that silicon nitride, barium hydroxide and bonding agent, described silicon nitride, barium hydroxide and bonding agent add after deionized water stirring forms Mag and forms the first nitration case 3 by brushing mode.
The preferred embodiment of the invention also has, and described bonding agent is polyhydric alcohol.
The preferred embodiment of the invention also has, and the weight ratio of described silicon nitride, barium hydroxide, bonding agent and deionized water is 100:3:17:12.
The preferred embodiment of the invention also has, and described second oxide layer 4 is silicon oxide, and described silicon oxide is reacted with hyperoxia agent by silicon nitride to be made, and described hyperoxia agent is concentrated sulphuric acid.
Further preferred embodiment of the present invention also has, and the silicon oxide of described second oxide layer 4 uses lance ejection, and the spray speed scope of described spray gun is 11km/h, and the jet length scope away from injected is 30 cm.
The preferred embodiment of the invention also has, at the inner surface that surface is crucible of described crucible body 1 and upper end bead.
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 is also covered with the first silicon nitride layer 3 on the lateral wall of described crucible body 1.
The brushing method of a kind of coating based on above-mentioned high-purity coating type polysilicon crucible, comprises the following steps:
S1, polysilicon crucible body is processed into the surface being evenly equipped with several pits or annular groove；
S2, the first nitration case of brushing Mag on the surface of the polysilicon crucible body being evenly equipped with several pits, and make the first nitration case be filled in several pits described or annular groove；
S3, described Mag first nitration case condense before, described first nitration case surface spray granular second oxide layer；
S4, the most again to granular second vaporific the 3rd nitration case of oxide layer surface injection, until the 3rd vaporific nitration case is completely covered granular second oxide layer；
S5, high temperature sintering, until the first nitration case of Mag, the second oxide layer and the 3rd nitration case condense completely and become an overall structure with polysilicon crucible body.
The preferred embodiment of the invention is, in described step S2, described first nitration case includes that silicon nitride, barium hydroxide and bonding agent, described silicon nitride, barium hydroxide and bonding agent add deionized water stirring and form Mag.
The preferred embodiment of the invention also has, and in described step S3, described second oxide layer is granular silicon oxide, and the granular size scope of described silicon oxide is 6mm2, described granular silicon oxide uses lance ejection to the surface of the first nitration case of Mag.
The preferred embodiment of the invention also has, and in described step S4, after described the 3rd vaporific nitration case injection is completely covered the second oxide layer granule, then by rubber, the 3rd nitration case above the second oxide layer granule is polished into smooth plane.
Preferably 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, including crucible body 1, it is evenly equipped with several annular grooves on the surface of described crucible body 1, is attached with the first nitration case the 3, second oxide layer 4 and the 3rd nitration case 5 on the described surface being evenly equipped with several annular grooves successively；
Described first nitration case 3 is by brushing mode, and by the silicon nitride coated of Mag in the surface of the crucible basis being evenly equipped with several annular grooves, the coating thickness scope of described first nitration case 3 is 15mm；
Described second oxide layer 4 is the silicon oxide of powder, by spray regime, the silicon oxide of powder is sprayed the first nitration case 3 surface in the Mag not yet condensed, and described second oxide layer 4 forms graininess on the surface of the first nitration case 3；
Described 3rd nitration case 5 is vaporific silicon nitride, and by spraying method by vaporific silicon nitride spray finishing in the surface of the second oxide layer 4, until the granule of described second oxide layer 4 is capped, described 3rd nitration case 5 forms shiny surface.
The preferred embodiment of the invention is, described first nitration case 3 includes that silicon nitride, barium hydroxide and bonding agent, described silicon nitride, barium hydroxide and bonding agent add after deionized water stirring forms Mag and forms the first nitration case 3 by brushing mode.
The preferred embodiment of the invention also has, and described bonding agent is organic polyethylene alcohol.
The preferred embodiment of the invention also has, and the weight ratio of described silicon nitride, barium hydroxide, bonding agent and deionized water is 100:4:18:13.
The preferred embodiment of the invention also has, and described second oxide layer 4 is silicon oxide, and described silicon oxide is reacted with hyperoxia agent by silicon nitride 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 oxide layer 4 uses lance ejection, and the spray speed scope of described spray gun is 15km/h, and the jet length scope away from injected is 40 cm.
The preferred embodiment of the invention also has, at the inner surface that surface is crucible of described crucible body 1 and upper end bead.
Further preferred embodiment of the present invention also has, and the shape of cross section of described annular groove 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 is also covered with the first silicon nitride layer 3 on the lateral wall of described crucible body 1.
The brushing method of a kind of coating based on above-mentioned high-purity coating type polysilicon crucible, comprises the following steps:
S1, polysilicon crucible body is processed into the surface being evenly equipped with several pits or annular groove；
S2, the first nitration case of brushing Mag on the surface of the polysilicon crucible body being evenly equipped with several pits, and make the first nitration case be filled in several pits described or annular groove；
S3, described Mag first nitration case condense before, described first nitration case surface spray granular second oxide layer；
S4, the most again to granular second vaporific the 3rd nitration case of oxide layer surface injection, until the 3rd vaporific nitration case is completely covered granular second oxide layer；
S5, high temperature sintering, until the first nitration case of Mag, the second oxide layer and the 3rd nitration case condense completely and become an overall structure with polysilicon crucible body.
The preferred embodiment of the invention is, in described step S2, described first nitration case includes that silicon nitride, barium hydroxide and bonding agent, described silicon nitride, barium hydroxide and bonding agent add deionized water stirring and form Mag.
The preferred embodiment of the invention also has, and in described step S3, described second oxide layer is granular silicon oxide, and the granular size scope of described silicon oxide is 8mm2, described granular silicon oxide uses lance ejection to the surface of the first nitration case of Mag.
The preferred embodiment of the invention also has, and in described step S4, after described the 3rd vaporific nitration case injection is completely covered the second oxide layer granule, then by rubber, the 3rd nitration case above the second oxide layer granule is polished into smooth plane.
Preferably 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, including crucible body 1, it is evenly equipped with annular groove on the surface of described crucible body 1, is attached with the first nitration case the 3, second oxide layer and 4 the 3rd nitration cases 5 on the described surface being evenly equipped with several annular grooves successively；
Described first nitration case is by brushing mode, and by the silicon nitride coated of Mag in the surface of the crucible body 1 being evenly equipped with several annular grooves, the coating thickness scope of described first nitration case 3 is 19 mm；
Described second oxide layer 4 is the silicon oxide of powder, by spray regime, the silicon oxide of powder is sprayed the first nitration case surface in the Mag not yet condensed, and described second oxide layer 4 forms graininess on the surface of the first nitration case 3；
Described 3rd nitration case 5 is vaporific silicon nitride, and by spraying method by vaporific silicon nitride spray finishing in the second oxide layer 4 surface, until the granule of described second oxide layer 4 is capped, described 3rd nitration case 5 forms shiny surface.
The preferred embodiment of the invention is, described first nitration case 3 includes that silicon nitride, barium hydroxide and bonding agent, described silicon nitride, barium hydroxide and bonding agent add after deionized water stirring forms Mag and forms the first nitration case 3 by brushing mode.
The preferred embodiment of the invention also has, and described bonding agent is for there being acrylate.
The preferred embodiment of the invention also has, and the weight ratio of described silicon nitride, barium hydroxide, bonding agent and deionized water is 100:5:25:14.
The preferred embodiment of the invention also has, and described second oxide layer 4 is silicon oxide, and described silicon oxide is reacted with hyperoxia agent by silicon nitride to be made, and described hyperoxia agent is Neutral potassium chromate.
Further preferred embodiment of the present invention also has, and the silicon oxide of described second oxide layer 4 uses lance ejection, and the spray speed scope of described spray gun is 18km/h, and the jet length scope away from injected is 80 cm.
The preferred embodiment of the invention also has, at the inner surface that surface is crucible of described crucible body 1 and upper end bead.
Further preferred embodiment of the present invention also has, and the shape of cross section of described annular groove 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 is also covered with the first silicon nitride layer 3 on the lateral wall of described crucible body 1.
The brushing method of a kind of coating based on above-mentioned high-purity coating type polysilicon crucible, comprises the following steps:
S1, polysilicon crucible body is processed into the surface being evenly equipped with several pits or annular groove；
S2, the first nitration case of brushing Mag on the surface of the polysilicon crucible body being evenly equipped with several pits, and make the first nitration case be filled in several pits described or annular groove；
S3, described Mag first nitration case condense before, described first nitration case surface spray granular second oxide layer；
S4, the most again to granular second vaporific the 3rd nitration case of oxide layer surface injection, until the 3rd vaporific nitration case is completely covered granular second oxide layer；
S5, high temperature sintering, until the first nitration case of Mag, the second oxide layer and the 3rd nitration case condense completely and become an overall structure with polysilicon crucible body.
The preferred embodiment of the invention is, in described step S2, described first nitration case includes that silicon nitride, barium hydroxide and bonding agent, described silicon nitride, barium hydroxide and bonding agent add deionized water stirring and form Mag.
The preferred embodiment of the invention also has, and in described step S3, described second oxide layer is granular silicon oxide, and the granular size scope of described silicon oxide is 10mm2, described granular silicon oxide uses lance ejection to the surface of the first nitration case of Mag.
The preferred embodiment of the invention also has, and in described step S4, after described the 3rd vaporific nitration case injection is completely covered the second oxide layer granule, then by rubber, the 3rd nitration case above the second oxide layer granule is polished into smooth plane.
Preferably 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, including crucible body 1, it is evenly equipped with several annular grooves on the surface of described crucible body 1, is attached with the first nitration case the 3, second oxide layer 4 and the 3rd nitration case 5 on the described surface being evenly equipped with several annular grooves successively；
Described first nitration case 3 is by brushing mode, and by the silicon nitride coated of Mag in the surface of the crucible basis being evenly equipped with several annular grooves, the coating thickness scope of described first nitration case 3 is 20 mm；
Described second oxide layer 4 is the silicon oxide of powder, by spray regime, the silicon oxide of powder is sprayed the first nitration case 3 surface in the Mag not yet condensed, and described second oxide layer 4 forms graininess on the surface of the first nitration case 3；
Described 3rd nitration case 5 is vaporific silicon nitride, and by spraying method by vaporific silicon nitride spray finishing in the surface of the second oxide layer 4, until the granule of described second oxide layer 4 is capped, described 3rd nitration case 5 forms shiny surface.
The preferred embodiment of the invention is, described first nitration case 3 includes that silicon nitride, barium hydroxide and bonding agent, described silicon nitride, barium hydroxide and bonding agent add after deionized water stirring forms Mag and forms the first nitridation 3 by brushing mode.
The preferred embodiment of the invention also has, and described bonding agent is acrylate.
The preferred embodiment of the invention also has, and the weight ratio of described silicon nitride, barium hydroxide, bonding agent and deionized water is 100:5:30:15.
The preferred embodiment of the invention also has, and described second oxide layer 4 is silicon oxide, and described silicon oxide is reacted with hyperoxia agent by silicon nitride 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 oxide layer 4 uses lance ejection, and the spray speed scope of described spray gun is 20km/h, and the jet length scope away from injected is 100 cm.
The preferred embodiment of the invention also has, at the inner surface that surface is crucible of described crucible body 1 and upper end bead.
Further preferred embodiment of the present invention also has, and the shape of cross section of described annular groove 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 3 m, and width range is 1 m.
Further preferred embodiment of the present invention also has, and is also covered with the first silicon nitride layer 3 on the lateral wall of described crucible body 1.
The brushing method of a kind of coating based on above-mentioned high-purity coating type polysilicon crucible, comprises the following steps:
S1, polysilicon crucible body is processed into the surface being evenly equipped with several pits or annular groove；
S2, the first nitration case of brushing Mag on the surface of the polysilicon crucible body being evenly equipped with several pits, and make the first nitration case be filled in several pits described or annular groove；
S3, described Mag first nitration case condense before, described first nitration case surface spray granular second oxide layer；
S4, the most again to granular second vaporific the 3rd nitration case of oxide layer surface injection, until the 3rd vaporific nitration case is completely covered granular second oxide layer；
S5, high temperature sintering, until the first nitration case of Mag, the second oxide layer and the 3rd nitration case condense completely and become an overall structure with polysilicon crucible body.
The preferred embodiment of the invention is, in described step S2, described first nitration case includes that silicon nitride, barium hydroxide and bonding agent, described silicon nitride, barium hydroxide and bonding agent add deionized water stirring and form Mag.
The preferred embodiment of the invention also has, and in described step S3, described second oxide layer is granular silicon oxide, and the granular size scope of described silicon oxide is 10mm2, described granular silicon oxide uses lance ejection to the surface of the first nitration case of Mag.
The preferred embodiment of the invention also has, and in described step S4, after described the 3rd vaporific nitration case injection is completely covered the second oxide layer granule, then by rubber, the 3rd nitration case above the second oxide layer granule is polished into smooth plane.
Preferably 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, on the premise of without departing from the technology of the present invention principle; can also make some improvements and modifications, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (10)
1. a high-purity coating type polysilicon crucible, including crucible body (1), it is characterized in that, several pits or annular groove (2) it is evenly equipped with on the surface of described crucible body (1), the first nitration case (3), the second oxide layer (4) and the 3rd nitration case (5) it is attached with successively on the described surface being evenly equipped with several pits or annular groove, at the inner surface that surface is crucible of described crucible body (1) and upper end bead, the shape of cross section of described pit be the shape of cross section of Ω ring connected in star be dove-tail；
Described first nitration case (3) is by brushing mode, by the silicon nitride coated of Mag in the surface of the crucible body (1) being evenly equipped with several pits or annular groove (2), the coating thickness scope of described first nitration case (3) is 2 ~ 20 mm；
Described second oxide layer (3) is the silicon oxide of powder, by spray regime, the silicon oxide of powder being sprayed the first nitration case (3) surface in the Mag not yet condensed, described second oxide layer (4) forms graininess on the surface of the first nitration case (2)；
Described 3rd nitration case (5) is vaporific silicon nitride, by spraying method by vaporific silicon nitride spray finishing in the surface of the second oxide layer (4), until the granule of described second oxide layer (4) is capped, described 3rd nitration case (5) forms shiny surface.
High-purity coating type polysilicon crucible the most as claimed in claim 1, it is characterized in that, described first nitration case (3) includes silicon nitride, barium hydroxide and bonding agent, described silicon nitride, barium hydroxide and bonding agent form the first nitration case (2) by brushing mode after adding deionized water stirring formation Mag, the silicon oxide of described second oxide layer (4) uses lance ejection, the spray speed scope of described spray gun is 5 ~ 20 km/h, and the jet length scope away from injected is 20 ~ 100 cm.
High-purity coating type polysilicon crucible the most as claimed in claim 2, it is characterised in that described bonding agent is the one in organosilan, silicic acid, polyhydric alcohol, polyvinyl alcohol and acrylate.
High-purity coating type polysilicon crucible the most as claimed in claim 2, it is characterised in that the weight ratio of described silicon nitride, barium hydroxide, bonding agent and deionized water is 100:5 ~ 1:15 ~ 30:8 ~ 15.
High-purity coating type polysilicon crucible the most as claimed in claim 1, it is characterized in that, described second oxide layer (4) is silicon oxide, described silicon oxide is reacted with hyperoxia agent by silicon nitride to be made, and described hyperoxia agent is any one in hydrogen peroxide, ozone, concentrated sulphuric acid, nitric acid, Neutral potassium chromate, potassium permanganate.
6. the brushing method of a coating based on coating type polysilicon crucible high-purity described in any one in claim 1-5, it is characterised in that comprise the following steps:
S1, polysilicon crucible body (1) is processed into it is evenly equipped with several pits or the surface of annular groove (2)；
S2, first nitration case (3) of brushing Mag on the surface of the polysilicon crucible body (1) being evenly equipped with several pits (2) or annular groove, and make the first nitration case (3) be filled in several pits described or annular groove (2)；
S3, described Mag the first nitration case (3) condense before, described first nitration case (3) surface spray granular second oxide layer (4)；
S4, the most again to vaporific the 3rd nitration case (5) of granular second oxide layer (4) surface injection, until the 3rd vaporific nitration case (5) is completely covered granular second oxide layer (4)；
S5, high temperature sintering, until first nitration case (3) of Mag, the second oxide layer (4) and the 3rd nitration case (5) condense completely and become an overall structure 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 nitration case (3) includes that silicon nitride, barium hydroxide and bonding agent, described silicon nitride, barium hydroxide and bonding agent add deionized water stirring and form Mag.
8. the brushing method of coating as claimed in claim 6, it is characterised in that in described step S3, described second oxide layer (4) is granular silicon oxide, and the granular size scope of described silicon oxide is 2 ~ 10mm2, described granular silicon oxide uses lance ejection to the surface of first nitration case (3) of Mag.
9. the brushing method of coating as claimed in claim 6, it is characterized in that, in described step S4, after described the 3rd vaporific nitration case (5) injection is completely covered the second oxide layer (4) granule, then by rubber, the 3rd nitration case (5) above the second oxide layer (4) granule is polished into smooth plane.
10. the brushing method of the coating as described in any one in claim 6 to 9, it is characterised in that in described step S5, described sintering range is 80 ~ 200 DEG C.
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| CN101213328A (en) * | 2005-07-01 | 2008-07-02 | 维苏维尤斯·克鲁斯布公司 | Crucible for the crystallization of silicon |
| CN101942693A (en) * | 2009-07-08 | 2011-01-12 | 合晶科技股份有限公司 | Quartz glass crucible with protective layer and manufacturing method thereof |
| CN104562192A (en) * | 2015-01-30 | 2015-04-29 | 扬州荣德新能源科技有限公司 | Casting method for polycrystalline silicon ingot |
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| JPH0597571A (en) * | 1991-06-13 | 1993-04-20 | Toshiba Ceramics Co Ltd | Crucible for pulling up silicon single crystal |
| JP3194547B2 (en) * | 1992-12-04 | 2001-07-30 | キヤノン株式会社 | Method for manufacturing polycrystalline silicon layer |
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| CN101213328A (en) * | 2005-07-01 | 2008-07-02 | 维苏维尤斯·克鲁斯布公司 | Crucible for the crystallization of silicon |
| CN101942693A (en) * | 2009-07-08 | 2011-01-12 | 合晶科技股份有限公司 | Quartz glass crucible with protective layer and manufacturing method thereof |
| CN104562192A (en) * | 2015-01-30 | 2015-04-29 | 扬州荣德新能源科技有限公司 | Casting method for polycrystalline silicon ingot |
| CN204530023U (en) * | 2015-01-30 | 2015-08-05 | 扬州荣德新能源科技有限公司 | A kind of crucible producing polysilicon |
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