CN101508590B - Crucible pot coating for polysilicon casting ingot and preparation method - Google Patents
Crucible pot coating for polysilicon casting ingot and preparation method Download PDFInfo
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- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 2
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Landscapes
- Silicon Compounds (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to a crucible coating, in particular to a ceramic crucible coating used in producing polycrystalline silicon cast ingot, and also relates to a preparation method of ceramic crucible coating used for polycrystalline silicon cast ingot. The solid content in the formulation of the crucible coating used for polycrystalline silicon cast ingot comprises 80-99% of silicon nitride and 1-20% of filming agent containing silicon element by weight percentage; after sintering the total oxygen content is 0.2-4.9% by weight percentage. The invention aims at providing a crucible coating used for polycrystalline silicon cast ingot and a preparation method; in the invention, a technique proposal in which the coating contains lower oxygen content is adopted as far as possible, so that potential pollution can be reduced, and meanwhile filming and spraying technologies are adopted to guarantee the stability of the silicon nitride layer and the quality of the silicon ingot in the use process of the crucible.
Description
Technical field
The present invention relates to a kind of crucible coating layer, particularly a kind of ceramic crucible coating specifically is applied in the polycrystalline silicon ingot casting production.The invention still further relates to the preparation method of a kind of polycrystalline silicon ingot casting with the ceramic crucible coating.
Background technology
Ceramic crucible is the crucial requisite during polycrystalline silicon ingot casting is produced, and mainly is to be used for splendid attire molten silicon liquid.The main chemical compositions of ceramic crucible is a silicon-dioxide, and selecting silicon-dioxide is that it has high purity and availability as the major cause of the material of crucible.Yet, adopt ceramic crucible to exist a lot of problems.
Silicon in the molten state can react with the ceramic crucible of its contact.Molten silicon and silicon dioxde reaction generate silicon monoxide, thereby introduce oxygen contamination silicon liquid.And silicon monoxide has volatility, can with the graphite member reaction in the polycrystalline silicon ingot or purifying furnace, generate silit and carbon monoxide.Carbon monoxide can generate more volatile matter or impurity with the molten silicon reaction again, like the carbide and the oxide compound of silicon monoxide, carbon, silit, metallic traces or additive.Carbon also can pollute silicon, and silicon also can with the various impurity in the ceramic crucible, react like iron, boron, aluminium etc.
Reaction between silicon-dioxide and the molten silicon impels silicon adhesion on crucible; Because the thermal expansivity between these two kinds of materials of silicon-dioxide and silicon is different; If silicon materials and ceramic crucible wall combine closely when crystal cools off, to cause crystalline silicon or ceramic crucible to break probably.The Long contact time of silicon melt and ceramic crucible also can cause the corrosion of ceramic crucible, even causes that crucible is damaged, causes silicon hydrorrhea stream.
In order to address these problems; The general inwall that adopts material such as silicon nitride to be coated in ceramic crucible as coating on the technology; Isolate silicon melt and contact, can prevent or reduce molten silicon and silicon dioxde reaction, avoid or reduce polycrystal silicon ingot and pollute and ftracture with the direct of ceramic crucible.In order to reach this effect, silicon nitride coating must have enough thickness to prevent that silicon and silicon-dioxide from reacting, and silicon nitride coating itself does not allow to introduce new contaminating impurity silicon.
But, adopt the ceramic crucible of silicon nitride coating still to have problems.Such as, reacting in order to prevent silicon and ceramic crucible, the thickness of required silicon nitride coating generally needs at about 200-300 μ m at least, so the silicon nitride coating operation is expensive and consuming time.In addition; This silicon nitride coating is also insecure; During use even before using, come off easily or peel off, can not prevent fully that silicon and silicon-dioxide from reacting, be prone to cause and glue crucible and split phenomenon such as ingot; And can not intercept effectively that impurity has influenced the quality of silicon ingot to the pollution of silicon ingot in the crucible.
In the various documents at home and abroad, proposed, attempted to solve the ceramic crucible silicon nitride coating and come off easily or peel off problem about difficult drop-off or stable silicon nitride coating crucible of peeling off and preparation method thereof.
Known technology about preparing stable crucible silicon nitride coating has: first kind is with silicon nitride coating oxidation under the controlled calcining cycle under 700 ℃-1450 ℃ high temperature; Second kind is in silicon nitride coating, to add sintering or bonding auxiliary, and additive can be for example Al of metal or oxide addition
2O
3, SiO
2, AlN, Al, Si, SILICA FUME or fine silica powder and other material.But the degree of oxidation and the oxygen level of the wayward silicon nitride of these methods, and generally need use hypoxic highly purified silicon nitride coating for high-quality polysilicon chip production; The third is to use chemical vapour deposition, solvent evaporation, high-temperature flame treatment and other costlinesses and complicated means to spray crucible coating layer.
Disclose a kind of crucibles in the USP of the patent No. 4741925 and used silicon nitride coating through chemical vapour deposition spraying under 1250 ℃; The patent No. is that the PCT patent of WO2004053207A1 discloses through the plasma spraying silicon nitride coating; Described in the USP of the patent No. 4218418 through rapid heating and in silica crucible, formed glass coating to prevent silicon rimose technology during melt processed.Though these methods can effectively prevent the problem that silicon nitride coating comes off or peels off, cost is too expensive, is inappropriate for aborning and promotes the use of.
A kind of silicon nitride coating with low oxygen content is disclosed in the USP of the patent No. 6165425; The oxygen level of this silicon nitride coating is the 0.3%-5% weight ratio; Also can comprise sticker such as polyoxyethylene glycol, and in preferred temperature is 500 ℃-700 ℃ and air atmosphere, carry out sintering.Under so low sintering temperature, silicon nitride is difficult to oxidized, can not form silicon-dioxide on the silicon nitride crystal boundary.Yet because there is not the oxidation of silicon nitride coating, this coating keeps powdery and when packing liquid-state silicon into crucible, is easy to impaired.
The patent No. is that the PCT patent of WO2007039310A1 discloses a kind of silicon nitride of the 80%-95% of including weight ratio, the low temperature mineral binder of 5%-20% weight ratio, and the oxygen level of this coating is 5%-15%.This technology is based on the oxygen that uses finite quantity or manipulated variable in the coating.Oxygen is introduced like collosol and gel, organometallic compound, nano particle, microfloc, non-miscible solutions, microemulsion, oxide compound mainly with low temperature mineral binder.In whole coating, produce the bonding phase of lesser temps, thereby the anti-mechanical wear property of raising protective coating also keeps the desired properties of silicon nitride simultaneously, coming off or peeling off risk of coating reduces greatly.Though this preparation method makes coming off of coating or peel off risk reduction has to a certain degree been arranged; But because this preparation only is alpha-silicon nitride powders and mineral binder bond to be carried out simple physics mix; Although improved the stability of silicon nitride coating to a certain extent, still also there be coming off or peeling off risk of coating; In addition, the oxygen level of this coating higher (being 5%-15%) can cause oxygen contamination to a certain degree to silicon ingot, influences the silicon ingot quality.
Summary of the invention
The object of the present invention is to provide a kind of crucible pot coating for polysilicon casting ingot and preparation method; Adopt the lower technical scheme of oxygen level in the coating as much as possible; To reduce pollution hidden trouble; Adopt the stability of film-coating technique and spraying technology guarantee silicon nitride layer simultaneously, guarantee the quality of silicon ingot in the crucible use.
Technical scheme of the present invention is:
A kind of crucible pot coating for polysilicon casting ingot; Wherein: solid content comprises the silicon nitride of 80-99% weight ratio in the composition of raw materials of described coating; The coating agent that contains element silicon of 1-20% weight ratio, total oxygen content is the 0.2-4.9% weight ratio in the coating of sintering aftershaping.
A kind of crucible pot coating for polysilicon casting ingot, wherein: described crucible is a quartz ceramic crucible.
A kind of crucible pot coating for polysilicon casting ingot, wherein: the thickness of silicon nitride coating is 100 μ m-800 μ m.
A kind of crucible pot coating for polysilicon casting ingot; Wherein: the described coating agent that contains element silicon can be the organometallic compound based on chemistry of silicones of silicon-dioxide, tetraethyl orthosilicate, tetraethoxysilane or its combination, also can be monox nanometer particle, the silicon oxide colloid that is suitable for forming suspensoid.
A kind of crucible pot coating for polysilicon casting ingot, wherein: the described coating agent that contains element silicon can be to contain silicate ion SiO
3 2-Mineral compound.
A kind of crucible pot coating for polysilicon casting ingot, wherein: contain silicate ion SiO
3 2-Mineral compound be water glass or water glass.
The preparation method of crucible pot coating for polysilicon casting ingot, wherein:
(1), take by weighing a certain amount of beta-silicon nitride powder particle, add in deionized water or deionized water and the alcoholic acid mixing solutions, dispersed with stirring is evenly subsequent use;
(2), in above-mentioned suspension-s, add the coating agent that contains element silicon; Drip acidic solution after the stirring and dissolving pH of suspension is adjusted to 1.0-5.0; Then temperature of reaction is set to 20～100 ℃, obtains the silicon nitride suspending liquid of coated with silica in reaction under the continuously stirring state after 1～3 hour;
(3), adopt spraying coating process that suspension-s is sprayed into inner surface of crucible, put into roaster then and carry out sintering, take out crucible from sintering oven after being cooled to room temperature, accomplish the preparation of crucible pot coating for polysilicon casting ingot.
A kind of preparation method of crucible pot coating for polysilicon casting ingot, wherein: described acidic solution can preferably have tartrate, acetate, Hydrocerol A, oxysuccinic acid for containing the organic acid of carboxyl, also can be nitric acid.
The preparation method of crucible pot coating for polysilicon casting ingot, wherein:
(1), take by weighing a certain amount of beta-silicon nitride powder particle, add in deionized water or deionized water and the alcoholic acid mixing solutions, dispersed with stirring is evenly subsequent use;
(2), in above-mentioned suspension-s, add the coating agent that contains element silicon; Drip basic soln after the stirring and dissolving pH of suspension is adjusted to 8.0-11.0; Then temperature of reaction is set to 20～100 ℃, obtains the silicon nitride suspending liquid of coated with silica in reaction under the continuously stirring state after 1～3 hour;
(3), adopt spraying coating process that suspension-s is sprayed into inner surface of crucible, put into roaster then and carry out sintering, take out crucible from sintering oven after being cooled to room temperature, accomplish the preparation of crucible pot coating for polysilicon casting ingot.
A kind of preparation method of crucible pot coating for polysilicon casting ingot, wherein: described basic soln can be an aminated compounds, and ammoniacal liquor is preferably arranged.
A kind of preparation method of crucible pot coating for polysilicon casting ingot, wherein: the step of the spraying coating process described in the step (3) is: crucible is positioned on the rotatable spraying frame; Rotate crucible on one side, with spray gun silicon nitride suspending liquid equably be coated in the internal surface of crucible on one side.
A kind of preparation method of crucible pot coating for polysilicon casting ingot, wherein: the agglomerating operation steps described in the step (3) is: will spray good crucible and place in the sintering oven, and under air atmosphere, carry out sintering; Insulation is 1-5 hour under 500 ℃ of-1200 ℃ of temperature.
A kind of crucible pot coating for polysilicon casting ingot; Wherein: described beta-silicon nitride powder particle grain size can be 100nm～1.0 μ m; Particle and the particle diameter that also can be particle diameter＜100nm is that the particulate of 10nm～5.0 μ m mixes, and wherein the particulate weight ratio of particle diameter＜100nm is 0-30%.
The roaster of putting into that the present invention relates to carries out the agglomerating processing condition and can be: 600-1100 ℃ was carried out sintering 2-3 hour.
Adopt the beta-silicon nitride powder particle of multiple different size particle diameter, can effectively improve the hardness and the density of crucible coating layer, prevent that crucible coating layer from coming off or the generation of peeling phenomenon.
The present invention adopts chemical coating means to increase the sticking power of silicon nitride coating and crucible, hardness and density.Silicon nitride particle must form effective chemically bonded with the ceramic crucible internal surface; Could be firm attached to the ceramic crucible surface; What prior art was mentioned all is some simple physics absorption or the high chemical Vapor deposition processs of preparation cost; Through the coating too high oxygen level that the simple physics adsorption method prepares, can pollute silicon.The present invention realizes between the silicon nitride particle through chemistry coating means and silicon nitride particle and the effective chemically bonded of ceramic crucible surface formation, has increased sticking power, hardness and the density of silicon nitride coating and crucible.
Principle of work of the present invention: utilize the coating agent that contains element silicon in hydrolysis in sour environment or alkaline environment under 20～100 ℃ the temperature; Form active very strong positive silicic acid nano particle; Positive silicic acid is prone to dehydration and forms silicon-dioxide; Perhaps directly adopt the coating agent that contains element silicon of silicon dioxide gel, under the certain reaction condition, obtain the silicon nitride suspending liquid of coated with silica.Simple relatively silica dioxide granule or silicon-containing compound and silicon nitride physical mixed can produce the silica dioxide granule agglomeration; Make the too high oxygen level of coating; Cause the silicon ingot downgrade, because the nano silicon that liquid phase generates among the present invention is evenly to be coated on the submicron order silicon nitride particle surface, the agglomeration between the silica dioxide granule is not serious; Thereby the coating oxygen level for preparing is low; Reduced the risk that silicon ingot is polluted, and preparation cost of the present invention is low, is suitable for promoting the use of aborning.
The implementation result of various technical schemes provided by the invention and prior art are relatively
The sticking power about top coat among the present invention is to use POSITEST to pull that method sticking power tester measures according to ASTMD4541.This tester draws pulling-out force to estimate adhesive force of coatings through receiving greatly most of can bear of this coating before measure separating, that is, use hydraulic pressure to be pulled away from the substrate the required power of coating of specified test diameter.This power is represented (KPa) with pressure.
Advantage of the present invention: coat one deck nanometer silicon dioxide particle on the silicon nitride particle surface through particle design and compounding technology; Increase the specific surface and the surface reaction active site of silicon nitride silica composite granules; Thereby strengthen the adsorptive power between silicon nitride and crucible surface, the silicon nitride particle, can also prevent the excess diffusion of block, thereby reach the appearance that prevents that the crucible silicon nitride coating from coming off or peeling off, glue crucible and split phenomenons such as ingot; And the coating oxygen level is low; Reduced the risk that silicon ingot is polluted, preparation cost of the present invention in addition is low, is suitable for promoting the use of aborning.
Embodiment
Embodiment 1, a kind of crucible pot coating for polysilicon casting ingot; Wherein: solid content comprises the silicon nitride of 80% weight ratio in the composition of raw materials of described coating; The coating agent that contains element silicon of 20% weight ratio, total oxygen content is 3% weight ratio in the coating of sintering aftershaping.
Embodiment 2, a kind of crucible pot coating for polysilicon casting ingot; Wherein: solid content comprises the silicon nitride of 85% weight ratio in the composition of raw materials of described coating; The coating agent that contains element silicon of 15% weight ratio, total oxygen content is 2% weight ratio in the coating of sintering aftershaping.
Embodiment 3, a kind of crucible pot coating for polysilicon casting ingot; Wherein: solid content comprises the silicon nitride of 88% weight ratio in the composition of raw materials of described coating; The coating agent that contains element silicon of 12% weight ratio, total oxygen content is 1.8% weight ratio in the coating of sintering aftershaping.
Embodiment 4, a kind of crucible pot coating for polysilicon casting ingot; Wherein: solid content comprises the silicon nitride of 90% weight ratio in the composition of raw materials of described coating; The coating agent that contains element silicon of 10% weight ratio, total oxygen content is 1.5% weight ratio in the coating of sintering aftershaping.
Embodiment 5, a kind of crucible pot coating for polysilicon casting ingot; Wherein: solid content comprises the silicon nitride of 95% weight ratio in the composition of raw materials of described coating; The coating agent that contains element silicon of 5% weight ratio, total oxygen content is 1% weight ratio in the coating of sintering aftershaping.
Embodiment 6, a kind of crucible pot coating for polysilicon casting ingot; Wherein: solid content comprises the silicon nitride of 99% weight ratio in the composition of raw materials of described coating; The coating agent that contains element silicon of 1% weight ratio, total oxygen content is 0.2% weight ratio in the coating of sintering aftershaping.
Embodiment 7, a kind of crucible pot coating for polysilicon casting ingot; Wherein: solid content comprises the silicon nitride of 90% weight ratio in the composition of raw materials of described coating; The coating agent that contains element silicon of 10% weight ratio, total oxygen content is 4.5% weight ratio in the coating of sintering aftershaping.
Embodiment 8, a kind of crucible pot coating for polysilicon casting ingot; Wherein: solid content comprises the silicon nitride of 85% weight ratio in the composition of raw materials of described coating; The coating agent that contains element silicon of 15% weight ratio, total oxygen content is 4.9% weight ratio in the coating of sintering aftershaping.
Embodiment 9, a kind of crucible pot coating for polysilicon casting ingot; Wherein: solid content comprises the silicon nitride of 95% weight ratio in the composition of raw materials of described coating; The coating agent that contains element silicon of 5% weight ratio, total oxygen content is 2% weight ratio in the coating of sintering aftershaping.
Embodiment 10, a kind of crucible pot coating for polysilicon casting ingot, wherein: described crucible is a quartz ceramic crucible, all the other are with any embodiment among the embodiment 1-9.
Embodiment 11, a kind of crucible pot coating for polysilicon casting ingot, wherein: the thickness of silicon nitride coating is 100 μ m,, all the other are with any embodiment among the embodiment 1-10.
Embodiment 12, a kind of crucible pot coating for polysilicon casting ingot, wherein: the thickness of silicon nitride coating is 200 μ m,, all the other are with any embodiment among the embodiment 1-10.
Embodiment 13, a kind of crucible pot coating for polysilicon casting ingot, wherein: the thickness of silicon nitride coating is 300 μ m,, all the other are with any embodiment among the embodiment 1-10.
Embodiment 14, a kind of crucible pot coating for polysilicon casting ingot, wherein: the thickness of silicon nitride coating is 400 μ m,, all the other are with any embodiment among the embodiment 1-10.
Embodiment 15, a kind of crucible pot coating for polysilicon casting ingot, wherein: the thickness of silicon nitride coating is 500 μ m,, all the other are with any embodiment among the embodiment 1-10.
Embodiment 16, a kind of crucible pot coating for polysilicon casting ingot, wherein: the thickness of silicon nitride coating is 600 μ m,, all the other are with any embodiment among the embodiment 1-10.
Embodiment 17, a kind of crucible pot coating for polysilicon casting ingot, wherein: the thickness of silicon nitride coating is 700 μ m,, all the other are with any embodiment among the embodiment 1-10.
Embodiment 18, a kind of crucible pot coating for polysilicon casting ingot, wherein: the thickness of silicon nitride coating is 800 μ m,, all the other are with any embodiment among the embodiment 1-10.
Embodiment 19, a kind of crucible pot coating for polysilicon casting ingot, wherein: the described coating agent that contains element silicon is a tetraethyl orthosilicate, all the other are with any embodiment of embodiment 1-6.
Embodiment 20, a kind of crucible pot coating for polysilicon casting ingot, wherein: the described coating agent that contains element silicon is a tetraethoxysilane, all the other are with any embodiment of embodiment 1-6.
Embodiment 21, a kind of crucible pot coating for polysilicon casting ingot, wherein: the described coating agent that contains element silicon can be a silicon sol, all the other are with any embodiment of embodiment 7-9.
Embodiment 22, a kind of crucible pot coating for polysilicon casting ingot, wherein: the described coating agent that contains element silicon can be to contain silicate ion SiO
3 2-Mineral compound, all the other are with any embodiment of embodiment 7-9.
Embodiment 23, a kind of crucible pot coating for polysilicon casting ingot, wherein: contain silicate ion SiO
3 2-Mineral compound be water glass, all the other are with embodiment 22.
Embodiment 24, a kind of crucible pot coating for polysilicon casting ingot, wherein: contain silicate ion SiO
3 2-Mineral compound be water glass, all the other are with embodiment 22.
Embodiment 25, like the preparation method of embodiment 1-embodiment 24 described any one crucible pot coating for polysilicon casting ingot, wherein:
(1), take by weighing a certain amount of beta-silicon nitride powder particle, add in deionized water and the alcoholic acid mixing solutions, dispersed with stirring is evenly subsequent use;
(2), in above-mentioned suspension-s, add tetraethyl orthosilicate; Drip tartrate after the stirring and dissolving pH of suspension is adjusted to 1.0; Then temperature of reaction is set to 20 ℃, obtains the silicon nitride suspending liquid of coated with silica in reaction under the continuously stirring state after 1 hour;
(3), adopt spraying coating process that suspension-s is sprayed into inner surface of crucible, put into roaster then and carried out sintering 2 hours at 600 ℃, take out crucible from sintering oven after being cooled to room temperature, accomplish the preparation of crucible pot coating for polysilicon casting ingot.
Embodiment 26, like the preparation method of embodiment 1-embodiment 24 described any one crucible pot coating for polysilicon casting ingot, wherein:
(1), take by weighing a certain amount of beta-silicon nitride powder particle, add in deionized water and the alcoholic acid mixing solutions, dispersed with stirring is evenly subsequent use;
(2), in above-mentioned suspension-s, add tetraethoxysilane; Drip acetate after the stirring and dissolving pH of suspension is adjusted to 2.0; Then temperature of reaction is set to 30 ℃, obtains the silicon nitride suspending liquid of coated with silica in reaction under the continuously stirring state after 1.5 hours;
(3), adopt spraying coating process that suspension-s is sprayed into inner surface of crucible, put into roaster then and carried out sintering 3 hours at 800 ℃, take out crucible from sintering oven after being cooled to room temperature, accomplish the preparation of crucible pot coating for polysilicon casting ingot.
Embodiment 27, like the preparation method of embodiment 1-embodiment 24 described any one crucible pot coating for polysilicon casting ingot, wherein:
(1), take by weighing a certain amount of beta-silicon nitride powder particle, add in the deionized water, dispersed with stirring is evenly subsequent use;
(2), in above-mentioned suspension-s, add silicon sol, drip Hydrocerol A after the stirring and dissolving pH of suspension is adjusted to 3.0, then temperature of reaction is set to 50 ℃, after reacting 2 hours the continuously stirring state under, obtain the silicon nitride suspending liquid of coated with silica;
(3), adopt spraying coating process that suspension-s is sprayed into inner surface of crucible, put into roaster then and carried out sintering 2 hours at 1100 ℃, take out crucible from sintering oven after being cooled to room temperature, accomplish the preparation of crucible pot coating for polysilicon casting ingot.
Embodiment 28, like the preparation method of embodiment 1-embodiment 24 described any one crucible pot coating for polysilicon casting ingot, wherein:
(1), take by weighing a certain amount of beta-silicon nitride powder particle, add in the deionized water, dispersed with stirring is evenly subsequent use;
(2), in above-mentioned suspension-s, add silicon sol, drip oxysuccinic acid after the stirring and dissolving pH of suspension is adjusted to 4.0, then temperature of reaction is set to 80 ℃, after reacting 2.5 hours the continuously stirring state under, obtain the silicon nitride suspending liquid of coated with silica;
(3), adopt spraying coating process that suspension-s is sprayed into inner surface of crucible, put into roaster then and carried out sintering 2 hours at 600 ℃, take out crucible from sintering oven after being cooled to room temperature, accomplish the preparation of crucible pot coating for polysilicon casting ingot.
Embodiment 29, like the preparation method of embodiment 1-embodiment 24 described any one crucible pot coating for polysilicon casting ingot, wherein:
(1), take by weighing a certain amount of beta-silicon nitride powder particle, add in the deionized water, dispersed with stirring is evenly subsequent use;
(2), in above-mentioned suspension-s, add water glass, dropping ammonia adjusts to 9.0 with pH of suspension after the stirring and dissolving, then temperature of reaction is set to 100 ℃, obtains the silicon nitride suspending liquid of coated with silica after 3 hours in reaction under the continuously stirring state;
(3), adopt spraying coating process that suspension-s is sprayed into inner surface of crucible, put into roaster then and carried out sintering 3 hours at 700 ℃, take out crucible from sintering oven after being cooled to room temperature, accomplish the preparation of crucible pot coating for polysilicon casting ingot.
The preparation method of embodiment 30, a kind of crucible pot coating for polysilicon casting ingot, wherein: described acidic solution can be for containing the organic acid of carboxyl, and all the other are with any embodiment among the embodiment 25-29.
Embodiment 31, like the preparation method of embodiment 1-embodiment 24 described crucible pot coating for polysilicon casting ingot, wherein: (1), take by weighing a certain amount of beta-silicon nitride powder particle, add in deionized water and the alcoholic acid mixing solutions, dispersed with stirring is evenly subsequent use;
(2), in above-mentioned suspension-s, add tetraethoxysilane, dropping ammonia adjusts to 8.0 with pH of suspension after the stirring and dissolving, then temperature of reaction is set to 80 ℃, obtains the silicon nitride suspending liquid of coated with silica after 3 hours in reaction under the continuously stirring state;
(3), adopt spraying coating process that suspension-s is sprayed into inner surface of crucible, put into roaster then and carried out sintering 4 hours at 900 ℃, take out crucible from sintering oven after being cooled to room temperature, accomplish the preparation of crucible pot coating for polysilicon casting ingot.
Embodiment 32, like the preparation method of embodiment 1-embodiment 24 described crucible pot coating for polysilicon casting ingot, wherein:
(1), take by weighing a certain amount of beta-silicon nitride powder particle, add in the deionized water, dispersed with stirring is evenly subsequent use;
(2), in above-mentioned suspension-s, add silicon oxide colloid, dropping ammonia adjusts to 10.0 with pH of suspension after the stirring and dissolving, then temperature of reaction is set to 50 ℃, obtains the silicon nitride suspending liquid of coated with silica after 2 hours in reaction under the continuously stirring state;
(3), adopt spraying coating process that suspension-s is sprayed into inner surface of crucible, put into roaster then and carried out sintering 2 hours at 1100 ℃, take out crucible from sintering oven after being cooled to room temperature, accomplish the preparation of crucible pot coating for polysilicon casting ingot.
Embodiment 33, like the preparation method of embodiment 1-embodiment 24 described crucible pot coating for polysilicon casting ingot, wherein:
(1), take by weighing a certain amount of beta-silicon nitride powder particle, add in the deionized water, dispersed with stirring is evenly subsequent use;
(2), in above-mentioned suspension-s, add water glass, dropping ammonia adjusts to 10.0 with pH of suspension after the stirring and dissolving, then temperature of reaction is set to 100 ℃, obtains the silicon nitride suspending liquid of coated with silica after 1 hour in reaction under the continuously stirring state;
(3), adopt spraying coating process that suspension-s is sprayed into inner surface of crucible, put into roaster then and carry out sintering, take out crucible from sintering oven after being cooled to room temperature, accomplish the preparation of crucible pot coating for polysilicon casting ingot.
The preparation method of embodiment 34, a kind of crucible pot coating for polysilicon casting ingot, wherein: described basic soln can be an aminated compounds, all the other are with any embodiment among the embodiment 31-33.
The preparation method of embodiment 35, a kind of crucible pot coating for polysilicon casting ingot, wherein: the step of the spraying coating process described in the step (3) is: crucible is positioned on the rotatable spraying frame; Rotate crucible on one side, with spray gun silicon nitride suspending liquid equably be coated in the internal surface of crucible on one side, all the other are with any embodiment among embodiment 25-29 and the embodiment 31-33.
The preparation method of embodiment 36, a kind of crucible pot coating for polysilicon casting ingot, wherein: the agglomerating operation steps described in the step (3) is: will spray good crucible and place in the sintering oven, and under air atmosphere, carry out sintering; Insulation is 5 hours under 500 ℃ of temperature, and all the other are with any embodiment among embodiment 25-29 and the embodiment 31-33.
The preparation method of embodiment 37, a kind of crucible pot coating for polysilicon casting ingot, wherein: the agglomerating operation steps described in the step (3) is: will spray good crucible and place in the sintering oven, and under air atmosphere, carry out sintering; Insulation is 3 hours under 800 ℃ of temperature, and all the other are with any embodiment among embodiment 25-29 and the embodiment 31-33.
The preparation method of embodiment 38, a kind of crucible pot coating for polysilicon casting ingot, wherein: the agglomerating operation steps described in the step (3) is: will spray good crucible and place in the sintering oven, and under air atmosphere, carry out sintering; Insulation is 2 hours under 1000 ℃ of temperature, and all the other are with any embodiment among embodiment 25-29 and the embodiment 31-33.
The preparation method of embodiment 39, a kind of crucible pot coating for polysilicon casting ingot, wherein: the agglomerating operation steps described in the step (3) is: will spray good crucible and place in the sintering oven, and under air atmosphere, carry out sintering; Insulation is 1 hour under 1200 ℃ of temperature, and all the other are with any embodiment among embodiment 25-29 and the embodiment 31-33.
Embodiment 40, a kind of crucible pot coating for polysilicon casting ingot, wherein: described beta-silicon nitride powder particle grain size is 100nm～1.0 μ m, all the other are with any embodiment among the embodiment 1-9.
Embodiment 41, a kind of crucible pot coating for polysilicon casting ingot; Wherein: the particle that described beta-silicon nitride powder particle is particle diameter＜100nm and particle diameter are that the particulate of 10nm～5.0 μ m mixes; Wherein the particulate weight ratio of particle diameter＜100nm is 30%, and all the other are with any embodiment among the embodiment 1-9.
Embodiment 42, a kind of crucible pot coating for polysilicon casting ingot; Wherein: the particle that described beta-silicon nitride powder particle is particle diameter＜100nm and particle diameter are that the particulate of 10nm～5.0 μ m mixes; Wherein the particulate weight ratio of particle diameter＜100nm is 20%, and all the other are with any embodiment among the embodiment 1-9.
Embodiment 43, a kind of crucible pot coating for polysilicon casting ingot; Wherein: the particle that described beta-silicon nitride powder particle is particle diameter＜100nm and particle diameter are that the particulate of 10nm～5.0 μ m mixes; Wherein the particulate weight ratio of particle diameter＜100nm is 10%, and all the other are with any embodiment among the embodiment 1-9.
Embodiment 44, a kind of crucible pot coating for polysilicon casting ingot; Wherein: the particle that described beta-silicon nitride powder particle is particle diameter＜100nm and particle diameter are that the particulate of 10nm～5.0 μ m mixes; Wherein the particulate weight ratio of particle diameter＜100nm is 5%, and all the other are with any embodiment among the embodiment 1-9.
Embodiment 45, like the preparation method of embodiment 1-embodiment 24 described crucible pot coating for polysilicon casting ingot, wherein:
(1), take by weighing a certain amount of beta-silicon nitride powder particle, add in the deionized water, dispersed with stirring is evenly subsequent use;
(2), in above-mentioned suspension-s, add silicon oxide colloid, dropping ammonia adjusts to 11.0 with pH of suspension after the stirring and dissolving, then temperature of reaction is set to 20 ℃, obtains the silicon nitride suspending liquid of coated with silica after 2 hours in reaction under the continuously stirring state;
(3), adopt spraying coating process that suspension-s is sprayed into inner surface of crucible, put into roaster then and carry out sintering, take out crucible from sintering oven after being cooled to room temperature, accomplish the preparation of crucible pot coating for polysilicon casting ingot.
Claims (11)
1. crucible pot coating for polysilicon casting ingot; It is characterized in that: solid content comprises the silicon nitride of 80-99% weight ratio in the composition of raw materials of described coating; The coating agent that contains element silicon of 1-20% weight ratio, total oxygen content is the 0.2-4.9% weight ratio in the coating of sintering aftershaping; The described coating agent that contains element silicon is silicon-dioxide, tetraethyl orthosilicate, tetraethoxysilane, be suitable for forming wherein any one of the monox nanometer particle of suspensoid, silicon oxide colloid; Wherein the preparation method of crucible pot coating for polysilicon casting ingot is following:
(1), take by weighing a certain amount of beta-silicon nitride powder particle, add in deionized water or deionized water and the alcoholic acid mixing solutions, dispersed with stirring is evenly subsequent use;
(2), in above-mentioned suspension-s, add the coating agent that contains element silicon; Drip acidic solution after the stirring and dissolving pH of suspension is adjusted to 1.0-5.0; Then temperature of reaction is set to 20～100 ℃, obtains the silicon nitride suspending liquid of coated with silica in reaction under the continuously stirring state after 1～3 hour;
(3), adopt spraying coating process that suspension-s is sprayed into inner surface of crucible, put into roaster then and carry out sintering, take out crucible from sintering oven after being cooled to room temperature, accomplish the preparation of crucible pot coating for polysilicon casting ingot.
2. a kind of crucible pot coating for polysilicon casting ingot as claimed in claim 1 is characterized in that: described crucible is a quartz ceramic crucible.
3. a kind of crucible pot coating for polysilicon casting ingot as claimed in claim 1 is characterized in that: the thickness of silicon nitride coating is 100 μ m-800 μ m.
4. a kind of crucible pot coating for polysilicon casting ingot as claimed in claim 1 is characterized in that: the described coating agent that contains element silicon is to contain silicate ion SiO
3 2-Mineral compound.
5. a kind of crucible pot coating for polysilicon casting ingot as claimed in claim 4 is characterized in that: contain silicate ion SiO
3 2-Mineral compound be water glass.
6. a kind of crucible pot coating for polysilicon casting ingot as claimed in claim 1 is characterized in that: described acidic solution is the organic acid that contains carboxyl.
7. a kind of crucible pot coating for polysilicon casting ingot as claimed in claim 1; It is characterized in that: described beta-silicon nitride powder particle grain size is 100nm～1.0 μ m; Or the particle of particle diameter＜100nm and particle diameter are that the particulate of 10nm～5.0 μ m mixes, and wherein the particulate weight ratio of particle diameter＜100nm is 0-30%.
8. the preparation method of crucible pot coating for polysilicon casting ingot; It is characterized in that: solid content comprises the silicon nitride of 80-99% weight ratio in the composition of raw materials of described coating; The coating agent that contains element silicon of 1-20% weight ratio, total oxygen content is the 0.2-4.9% weight ratio in the coating of sintering aftershaping; The described coating agent that contains element silicon is silicon-dioxide, tetraethyl orthosilicate, tetraethoxysilane, be suitable for forming wherein any one of the monox nanometer particle of suspensoid, silicon oxide colloid; Wherein the preparation method of crucible pot coating for polysilicon casting ingot is following:
(1), take by weighing a certain amount of beta-silicon nitride powder particle, add in deionized water or deionized water and the alcoholic acid mixing solutions, dispersed with stirring is evenly subsequent use;
(2), in above-mentioned suspension-s, add the coating agent that contains element silicon; Drip basic soln after the stirring and dissolving pH of suspension is adjusted to 8.0-11.0; Then temperature of reaction is set to 20～100 ℃, obtains the silicon nitride suspending liquid of coated with silica in reaction under the continuously stirring state after 1～3 hour;
(3), adopt spraying coating process that suspension-s is sprayed into inner surface of crucible, put into roaster then and carry out sintering, take out crucible from sintering oven after being cooled to room temperature, accomplish the preparation of crucible pot coating for polysilicon casting ingot.
9. the preparation method of a kind of crucible pot coating for polysilicon casting ingot as claimed in claim 8, it is characterized in that: described basic soln is an aminated compounds.
10. the preparation method of a kind of crucible pot coating for polysilicon casting ingot as claimed in claim 8, it is characterized in that: the step of the spraying coating process described in the step (3) is: crucible is positioned on the rotatable spraying frame; Rotate crucible on one side, with spray gun silicon nitride suspending liquid equably be coated in the internal surface of crucible on one side.
11. the preparation method of a kind of crucible pot coating for polysilicon casting ingot as claimed in claim 8 is characterized in that: the agglomerating operation steps described in the step (3) is: will spray good crucible and place in the sintering oven, and under air atmosphere, carry out sintering; Insulation is 1-5 hour under 500 ℃ of-1200 ℃ of temperature.
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| US20130247818A1 (en) * | 2011-05-25 | 2013-09-26 | Saint-Gobain Research (Shanghai) Co., Ltd. | Silica crucible and method for fabricating the same |
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| CN115433480A (en) * | 2022-10-21 | 2022-12-06 | 广东华葆新材料科技有限公司 | Lithium silicate-based antistatic inorganic wall coating and preparation method thereof |
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