CN102221293B - Preparation method of coating for melting crucible - Google Patents
Preparation method of coating for melting crucible Download PDFInfo
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- CN102221293B CN102221293B CN 201110152133 CN201110152133A CN102221293B CN 102221293 B CN102221293 B CN 102221293B CN 201110152133 CN201110152133 CN 201110152133 CN 201110152133 A CN201110152133 A CN 201110152133A CN 102221293 B CN102221293 B CN 102221293B
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- melting kettle
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Abstract
The invention belongs to the technical field of coating preparation. A preparation method of a coating for a melting crucible comprises the following steps of: pre-drying the melting crucible; preparing a suspension by adopting a PVP (Polyvinyl Pyrrolidone) absolute ethanol solution and silicon nitride; uniformly spraying the suspension on the inner wall of the melting crucible; and pre-burning the melting crucible with sprayed coating to form a silicon nitride coating with uniform thickness and compact structure on the inner wall of the melting crucible. The method has the advantages that: the melting crucible is pre-dried and cleaned before being sprayed to contribute to adhesion of the coating; the PVP absolute ethanol solution is added to the suspension of the coating, the absolute ethanol is evaporated after the crucible is dried, the adhesive PVP leads the coating to be adhered on the inner wall of the crucible, and the coating has higher adhesive force, so that the crucible is prevented from reacting with and adhering melt, smooth demolding of ingots is realized, impurities are prevented from entering melt, the purification effect of the melt is realized, and the using requirement for the coating in a casting process is fulfilled.
Description
Technical field
The invention belongs to the technical field of preparation coating, particularly a kind of on the melting kettle inwall method of spraying silicon nitride coating.
Background technology
Prepare in the ingot casting process in the metallurgical smelting removal of impurities, all need to use melting kettle, in industry, normally used melting kettle is quartz or graphite crucible, inevitably produces the reaction adhesion when molten metal bath contacts with crucible, and the impurity in crucible also can enter into silicon melt simultaneously.Reaction adhesion between crucible and metal, infiltration and diffusion meeting cause problem in the ingot casting knockout course, the danger that makes polycrystalline silicon ingot casting fracture be arranged or break.The impurity of high concentration will produce adverse influence to the various performances of ingot casting as C, O etc.Usually coating makes melt and the isolation of melting kettle wall on crucible, reduces the reaction adhesion and makes the smooth demoulding of ingot casting, and stop the impurity in crucible to enter in metal in casting process.
Si
3N
4Because its self-diffusion coefficient is low, high temperature resistant, chemical stability is good, is usually used to as the coating material in the polysilicon casting process.The preparation method of silicon nitride coating is a lot, but common complex process, cost is high.Application number is 200810243655.6 patent of invention employing silicon nitride particle and deionized water formation Mag liquation, under low pressure after the spraying, sintering forms silicon nitride coating, but what use in the method is that deionized water forms the emulsion state liquation, after sintering, the adhesive of coating and melting kettle is less, very easily come off in casting process, thereby can't reach the effect of coating.
Summary of the invention
The objective of the invention is to overcome above-mentioned not enough problem, a kind of preparation method of coating for melting crucible is provided, utilize PVP ethanol solution and silicon nitride to form suspension, after spraying, the silicon nitride coating adhesive of preparation is larger, even thickness, compact structure have satisfied the requirement of isolating crucible and melt in the ingot casting process.
The technical scheme that the present invention adopts for achieving the above object is: a kind of preparation method of coating for melting crucible, at first melting kettle is smoked pretreatment, then adopt PVP ethanol solution and silicon nitride configuration suspension, suspension evenly is sprayed at the melting kettle inwall, the melting kettle that will spray at last coating carries out preheating, can the melting kettle inwall obtain a layer thickness evenly, the silicon nitride coating of compact structure.
Preparation method's concrete steps of described coating for melting crucible are as follows:
First step melting kettle is smoked pretreatment: melting kettle is put in directional solidification furnace, is that 3-10Pa, temperature are to be incubated 1-2h under 600-1000 ℃ in vacuum, and the cold rear taking-up crucible of stove cleans the organic solvent of removing on inwall with acetone;
Second step configuration coating: be to add Si in the ethanol solution of 6%-15% to the PVP mass percent
3N
4Powder, stir about 1-2h is uniformly dispersed powder as far as possible, obtains the suspension of silicon nitride coating, set aside for use;
The 3rd step spray coating: the spray gun that cleans up is connected with the air compressor machine gas outlet, first sprays with the absolute ethyl alcohol examination, after whole passage is smooth and easy, with standing Si
3N
4The supernatant liquor of suspension is poured in spray gun, and the even backward melting kettle inwall of vaporific powder to be sprayed sprays, and constantly rotates the melting kettle angle in spraying process, until in appearance without till obvious dew point and even thickness;
The 4th step preheating: the melting kettle that will spray coating is placed in directional solidification furnace, is evacuated down to 3-10Pa, and 1-2h is heated to 800-1000 ℃, and stove is chilled to room temperature after insulation 1-2h at this temperature, forms the silicon nitride coating of compact structure.
Described melting kettle can be silica crucible, graphite crucible, Al
2O
3Crucible, SiC crucible or MgO crucible when wherein melting kettle is silica crucible, can saves first step melting kettle and smoke pretreated operation.
In described suspension, the PVP mass percent is ethanol solution and the Si of 6%-10%
3N
4The powder mass ratio is 0.3-1.0.
Described Si
3N
4The granularity of powder is the 10-300 micron.
The pressure of described air compressor gas outlet is 100-5000Pa.
The thickness of described silicon nitride coating is 0.5-2mm.
remarkable result of the present invention is before spraying, melting kettle to be smoked pretreatment and cleaning treatment, make crucible fine and close clean, be conducive to the adhesion of coating, add the PVP ethanol solution when configuration coating suspension, smoke rear absolute ethyl alcohol evaporation, binding agent PVP adheres to coating on the crucible inwall, the adhesive of coating is larger, be unlikely to come off in the metal bath casting process, thereby with melt and the isolation of crucible inwall, prevent the reaction adhesion of crucible and melt, realize the smooth demoulding of ingot casting, prevent that simultaneously impurity from entering liquation, realize the refining effect of melt, satisfied the instructions for use of casting process floating coat.
To sum up, this process is simple, can prepare that a kind of thickness is fine and close, adhesive is large, the silicon nitride coating of compact structure, has realized not coming off of coating, thus the purpose that melt and melting kettle are effectively isolated.
Description of drawings
Accompanying drawing 1 is the preparation method's of coating for melting crucible of the present invention flow chart.
The specific embodiment
Describe the present invention in detail below in conjunction with specific embodiments and the drawings, but the present invention is not limited to specific embodiment.
Embodiment 1
The first step is smoked pretreatment: select " three height " graphite crucible as the melt carrier, due to the impact in long-time placement and process, need to smoke processing to crucible, smoking processing procedure carries out in directional solidification furnace, be 5Pa, be incubated 1h under 800 ℃ in vacuum, the cold rear taking-up crucible of stove cleans the organic solvent of removing on inwall with acetone;
The suspension of second step configuration silicon nitride coating: adding the 30g granularity in the ethanol solution of 20g 8wt% PVP is the Si of 100 microns
3N
4Powder, stir about 2h is uniformly dispersed powder as far as possible, set aside for use;
The 3rd step spray coating: the spray gun that cleans up is connected with the air compressor machine gas outlet, is 500Pa with air pressure adjustment, first sprays with the absolute ethyl alcohol examination, after whole passage is smooth and easy, with standing Si
3N
4The supernatant liquor of suspension is poured in spray gun, for preventing that excessive powder from entering spray gun and blocking passage, can inject less a little suspensions at every turn.The even backward crucible inwall of vaporific powder to be sprayed sprays, to evenly carry out in spraying process, constantly rotate the crucible angle, until in appearance without obviously dew point and thickness evenly till, coating layer thickness was difficult for thinly also being difficult for blocked uply, crossed the thin isolation effect that can't fully play coating, blocked uply easily came off in the pretreatment in later stage and fusion process, can weaken the effect of coating equally, and after making melting, silicon ingot becomes more difficult with separating of crucible;
The 4th step preheating: the crucible that will spray coating carries out preheating, remove wherein residual liquid phase and organic principle, prevent after these compositions of fusion process enter into melt, the preheating process is carried out in directional solidification furnace, the graphite crucible that has sprayed coating is placed in directional solidification furnace, is evacuated down to 4Pa, 1h is heated to 800 ℃, stove is chilled to room temperature after insulation 1h at this temperature, and forming a layer thickness is the silicon nitride coating of the compact structure of 0.8mm.Crucible after preheating is placed in clean environment, avoids polluting and the entering of impurity.
Embodiment 2
The first step is smoked pretreatment: select Al
2O
3Crucible is as the melt carrier, due to the impact in long-time placement and process, need to smoke processing to crucible, smoking processing procedure carries out in directional solidification furnace, be 8Pa, be incubated 1h under 600 ℃ in vacuum, the cold rear taking-up crucible of stove cleans the organic solvent of removing on inwall with acetone;
The suspension of second step configuration silicon nitride coating: adding the 20g granularity in the ethanol solution of 10g 6wt% PVP is the Si of 130 microns
3N
4Powder, stir about 2h is uniformly dispersed powder as far as possible, set aside for use;
The 3rd step spray coating: the spray gun that cleans up is connected with the air compressor machine gas outlet, is 300Pa with air pressure adjustment, first sprays with the absolute ethyl alcohol examination, after whole passage is smooth and easy, with standing Si
3N
4The supernatant liquor of suspension is poured in spray gun, for preventing that excessive powder from entering spray gun and blocking passage, can inject less a little suspensions at every turn.The even backward crucible inwall of vaporific powder to be sprayed sprays, to evenly carry out in spraying process, constantly rotate the crucible angle, until in appearance without obviously dew point and thickness evenly till, coating layer thickness was difficult for thinly also being difficult for blocked uply, crossed the thin isolation effect that can't fully play coating, blocked uply easily came off in the pretreatment in later stage and fusion process, can weaken the effect of coating equally, and after making melting, silicon ingot becomes more difficult with separating of crucible;
The 4th step preheating: the crucible that will spray coating carries out preheating, remove wherein residual liquid phase and organic principle, prevent after these compositions of fusion process enter into melt, the preheating process is carried out in directional solidification furnace, the graphite crucible that has sprayed coating is placed in directional solidification furnace, is evacuated down to 6Pa, 2h is heated to 900 ℃, stove is chilled to room temperature after insulation 3h at this temperature, and forming a layer thickness is the silicon nitride coating of the compact structure of 0.6mm.Crucible after preheating is placed in clean environment, avoids polluting and the entering of impurity.
It is consistent through case test that the present invention prepares silicon nitride coating, and technique is simple, and coating performance is good, and energy consumption is little, and cost is low, and the cycle is short, and production efficiency is higher.
Claims (6)
1. the preparation method of a coating for melting crucible, it is characterized in that, at first melting kettle is smoked pretreatment, then adopt PVP ethanol solution and silicon nitride configuration suspension, suspension evenly is sprayed at the melting kettle inwall, the melting kettle that will spray at last coating carries out preheating, can the melting kettle inwall obtain a layer thickness evenly, the silicon nitride coating of compact structure; Concrete steps are as follows:
First step melting kettle is smoked pretreatment: melting kettle is put in directional solidification furnace, is that 3-10Pa, temperature are to be incubated 1-2h under 600-1000 ℃ in vacuum, and the cold rear taking-up crucible of stove cleans the organic solvent of removing on inwall with acetone;
Second step configuration coating: be to add Si in the ethanol solution of 6%-15% to the PVP mass percent
3N
4Powder, stir about 1-2h is uniformly dispersed powder as far as possible, obtains the suspension of silicon nitride coating, set aside for use;
The 3rd step spray coating: the spray gun that cleans up is connected with the air compressor machine gas outlet, first sprays with the absolute ethyl alcohol examination, after whole passage is smooth and easy, with standing Si
3N
4The supernatant liquor of suspension is poured in spray gun, and the even backward melting kettle inwall of vaporific powder to be sprayed sprays, and constantly rotates the melting kettle angle in spraying process, until in appearance without till obvious dew point and even thickness;
The 4th step preheating: the melting kettle that will spray coating is placed in directional solidification furnace, is evacuated down to 3-10Pa, and 1-2h is heated to 800-1000 ℃, and stove is chilled to room temperature after insulation 1-2h at this temperature, forms the silicon nitride coating of compact structure.
2. the preparation method of a kind of coating for melting crucible according to claim 1, is characterized in that, described melting kettle can be silica crucible, graphite crucible, Al
2O
3Crucible, SiC crucible or MgO crucible when wherein melting kettle is silica crucible, saves first step melting kettle and smoke pretreated operation.
3. the preparation method of a kind of coating for melting crucible according to claim 1, is characterized in that, in described suspension, the PVP mass percent is ethanol solution and the Si of 6%-10%
3N
4The powder mass ratio is 0.3-1.0.
4. the preparation method of a kind of coating for melting crucible according to claim 1, is characterized in that, described Si
3N
4The granularity of powder is the 10-300 micron.
5. the preparation method of a kind of coating for melting crucible according to claim 1, is characterized in that, the pressure of described air compressor machine gas outlet is 100-5000Pa.
6. the preparation method of a kind of coating for melting crucible according to claim 1, is characterized in that, the thickness of described silicon nitride coating is 0.5-2mm.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103130528B (en) * | 2011-12-05 | 2014-06-11 | 江苏协鑫硅材料科技发展有限公司 | Sintering-free crucible coating structure for ingot casting of polycrystalline silicon and manufacture method thereof |
| CN103132141A (en) * | 2011-12-05 | 2013-06-05 | 江苏协鑫硅材料科技发展有限公司 | Coating composition of graphite equipment used for polycrystalline silicon ingot furnace |
| CN102850086A (en) * | 2012-09-20 | 2013-01-02 | 光为绿色新能源股份有限公司 | Preparation method for ceramic crucible sintering-free coating for polysilicon ingot |
| CN103288357B (en) * | 2013-06-20 | 2016-03-30 | 天津英利新能源有限公司 | Silicon nitride solution and preparation method thereof, crucible used for polycrystalline silicon ingot casting and preparation method thereof |
| CN104668504B (en) * | 2013-11-30 | 2017-06-16 | 中国科学院金属研究所 | Non-crystaline amorphous metal component casting equipment and technique |
| CN104668503B (en) * | 2013-11-30 | 2017-05-31 | 中国科学院金属研究所 | A kind of non-crystaline amorphous metal component casting equipment and technique |
| CN105779912A (en) * | 2014-12-26 | 2016-07-20 | 比亚迪股份有限公司 | Method for prolonging service life of amorphous alloy smelting crucible and smelting method for amorphous alloy |
| CN104962991B (en) * | 2015-05-26 | 2018-04-17 | 江苏润弛太阳能材料科技有限公司 | A kind of silica crucible and preparation method thereof |
| CN105063757B (en) * | 2015-09-17 | 2017-12-29 | 晶科能源有限公司 | A kind of hypoxemia spraying method |
| DE102017204257A1 (en) | 2017-03-14 | 2018-09-20 | Schunk Kohlenstofftechnik Gmbh | Coated product and method of manufacture |
| CN107602139A (en) * | 2017-10-24 | 2018-01-19 | 陕西海恩得工贸有限公司 | A kind of material of melting titanium or titanium alloy crucible and the preparation method of crucible |
| TWI749334B (en) | 2019-06-24 | 2021-12-11 | 中美矽晶製品股份有限公司 | Crucible structure and method for forming isolating layer of crucible |
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| DE102006001162A1 (en) * | 2006-01-06 | 2007-07-12 | Labtec Gmbh | Patch cover for atopic dermatitis |
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