CN103920627A - Method for manufacturing polycrystal blowing crucibles for cast ingots - Google Patents
Method for manufacturing polycrystal blowing crucibles for cast ingots Download PDFInfo
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- CN103920627A CN103920627A CN201410176566.XA CN201410176566A CN103920627A CN 103920627 A CN103920627 A CN 103920627A CN 201410176566 A CN201410176566 A CN 201410176566A CN 103920627 A CN103920627 A CN 103920627A
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Abstract
The invention discloses a method for manufacturing polycrystal blowing crucibles for cast ingots. The method includes the steps that silicon nitride slurry is prepared; after 45%-60% by weight of silicon nitride powder, 1%-8% by weight of organic binding agents, 0-1.5% by weight of antioxidants and 40%-85% by weight of pure water are evenly mixed, the mixture is heated to be at 40 DEG C-100 DEG C; spraying is carried out, suspension liquid is sprayed on the surfaces of the crucibles with the spraying technology, the sprayed crucibles are continuously coated at 80 DEG C-100 DEG C, solidification is carried out for 1 hour-2 hours, and then cooling is carried out to enable the temperature to reach the indoor temperature. By means of the manufacturing method, the adsorbability of the surfaces of the crucibles is good, damage is not prone to being caused, high-temperature sintering is not needed, the oxidation pollution to the quartz crucibles and coatings is reduced, and energy consumption is reduced.
Description
Technical field
The present invention relates to the preparation method of polycrystalline blowing crucible for a kind of ingot casting.
Background technology
Quartz ceramic crucible be in polycrystalline silicon ingot casting process for loading the container of melting polycrystalline silicon raw material, mostly be square.When making and use, there are two problems in quartz ceramic crucible.
On the one hand, when loading melting polycrystalline silicon raw material, the polysilicon of molten condition can react with quartz ceramic crucible, be that silicon reacts generation SiO and oxygen with the main component SiO2 of quartz ceramic crucible, oxygen can pollute silicon, SiO has volatility, and by with stove in graphite member react, silicon monoxide reacts with graphite and forms carborundum and carbon monoxide.Then carbon monoxide forms other volatility silicon monoxide and carbon by reacting with molten silicon.
On the other hand, reacting between silica and silicon can promote adhering to of silicon and crucible.This adhere to silicon and vitreous silica bi-material between the difference of thermal coefficient of expansion combine and can in silicon ingot, produce stress.
Again because ceramic crucible surface need to have certain porosity, this pore can cause the bonding of silicon ingot and crucible and crucible impurity to the infiltration of silicon ingot.The bonding phenomenon of silicon ingot and silica crucible is that the coefficient of expansion due to silicon and vitreous silica has a long way to go, and silicon ingot, after cooling, can produce internal stress, can cause the cracking of silicon ingot when serious.The existence of pottery quartz crucible coating can solve silicon ingot in cooling rear generation internal stress and the problem that causes silicon ingot cracking.
According to current production experience and pertinent literature, record, the coating of silicon nitride is commonly used, the coating method of silicon nitride coating: manually air gun spraying, robot automatic coating, utilize swabbing to apply.
Summary of the invention
Goal of the invention: the present invention is directed to deficiency, propose a kind of crucible surface adsorptivity better, reduce silica crucible and coating oxidation pollutes, reduce the preparation method of polycrystalline blowing crucible for the ingot casting of energy consumption.
Technical scheme: the preparation method of polycrystalline blowing crucible for a kind of ingot casting of the present invention, the steps include:
(1) preparation Silicon Nitride: the silicon nitride powder that is 45-60% by mass fraction, mass fraction is the organic binder bond of 1-8%, mass fraction is the antioxidant of 0-1.5%, after the pure water that mass fraction is 40-85% mixes, is heated to 40-100 ° of C;
(2) spraying: adopt spraying coating process that suspension is sprayed to crucible surface, the crucible having sprayed is continued to proceed curing of coatings 1-2 hour under 80-100 ° of C condition, be then cooled to room temperature.
As preferably, described organic binder bond is polyvinyl chloride, polyacrylic acid, polyvinyl alcohol, sodium carboxymethylcellulose, polysaccharide polymer or any combination between them.
As preferably, described antioxidant is 2,6-di-t-butyl-4-methylphenol or ditert-butylhydro quinone.
As preferably, described spraying coating process adopts spray gun to spray, spray gun pressure is 20psi～40psi, spray distance is 25～30 centimetres, location land crucible width is 15～20 centimetres, in spraying process, a coating thickness is controlled at and is less than in 0.01mm, and crucible spraying temperature is in 40 ℃～65 ℃ controls.
Beneficial effect: preparation method of the present invention, crucible surface adsorptivity is better, is not subject to destruction; Do not need to carry out high temperature sintering, reduce silica crucible and coating oxidation and pollute, reduce energy consumption.
The specific embodiment
Below in conjunction with specific embodiment, the invention will be further described:
Embodiment 1
A preparation method for polycrystalline blowing crucible for ingot casting, the steps include:
(1) preparation Silicon Nitride: the silicon nitride powder that is 45% by mass fraction, mass fraction is 1% polyvinyl chloride, and mass fraction is 0.3% 2,6-di-t-butyl-4-methylphenol, mass fraction is, after 40% pure water mixes, to be heated to 40 ° of C;
(2) spraying: adopt spray gun to spray, spray gun pressure is 20ps, spray distance is 25 centimetres, location land crucible width is 15 centimetres, in spraying process, a coating thickness is controlled at and is less than in 0.01mm, crucible spraying temperature, in 40 ℃ of controls, continues the crucible having sprayed under 80 conditions, to proceed curing of coatings 1 hour, is then cooled to room temperature.
Embodiment 2
A preparation method for polycrystalline blowing crucible for ingot casting, the steps include:
(1) preparation Silicon Nitride: the silicon nitride powder that is 55% by mass fraction, the polyacrylic acid that mass fraction is 5%, mass fraction is 1% 2,6-di-t-butyl-4-methylphenol, after the pure water that mass fraction is 55% mixes, is heated to 70 ° of C;
(2) spraying: adopt spray gun to spray, spray gun pressure is 30psi, spray distance is 28 centimetres, location land crucible width is 17 centimetres, in spraying process, a coating thickness is controlled at and is less than in 0.01mm, crucible spraying temperature, in 50 ℃ of controls, continues the crucible having sprayed to proceed curing of coatings 1.5 hours under 90 ° of C conditions, is then cooled to room temperature.
Embodiment 3
A preparation method for polycrystalline blowing crucible for ingot casting, the steps include:
(1) preparation Silicon Nitride: the silicon nitride powder that is 60% by mass fraction, the sodium carboxymethylcellulose that mass fraction is 8%, the ditert-butylhydro quinone that mass fraction is 1.5%, after the pure water that mass fraction is 85% mixes, is heated to 100 ° of C;
(2) spraying: adopt spray gun to spray, spray gun pressure is 40psi, spray distance is 30 centimetres, location land crucible width is 20 centimetres, in spraying process, a coating thickness is controlled at and is less than in 0.01mm, crucible spraying temperature, in 65 ℃ of controls, continues the crucible having sprayed to proceed curing of coatings 2 hours under 100 ° of C conditions, is then cooled to room temperature.
Claims (4)
1. a preparation method for polycrystalline blowing crucible for ingot casting, the steps include:
(1) preparation Silicon Nitride: the silicon nitride powder that is 45-60% by mass fraction, mass fraction is the organic binder bond of 1-8%, mass fraction is the antioxidant of 0-1.5%, after the pure water that mass fraction is 40-85% mixes, is heated to 40-100 ° of C;
(2) spraying: adopt spraying coating process that suspension is sprayed to crucible surface, the crucible having sprayed is continued to proceed curing of coatings 1-2 hour under 80-100 ° of C condition, be then cooled to room temperature.
2. the preparation method of polycrystalline blowing crucible for a kind of ingot casting according to claim 1, is characterized in that: described organic binder bond is polyvinyl chloride, polyacrylic acid, polyvinyl alcohol, sodium carboxymethylcellulose, polysaccharide polymer or any combination between them.
3. the preparation method of polycrystalline blowing crucible for a kind of ingot casting according to claim 1, is characterized in that: described antioxidant is 2,6-di-t-butyl-4-methylphenol or ditert-butylhydro quinone.
4. the preparation method of polycrystalline blowing crucible for a kind of ingot casting according to claim 1, it is characterized in that: described spraying coating process adopts spray gun to spray, spray gun pressure is 20psi～40psi, spray distance is 25～30 centimetres, location land crucible width is 15～20 centimetres, in spraying process, a coating thickness is controlled at and is less than in 0.01mm, and crucible spraying temperature is in 40 ℃～65 ℃ controls.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410176566.XA CN103920627A (en) | 2014-04-29 | 2014-04-29 | Method for manufacturing polycrystal blowing crucibles for cast ingots |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410176566.XA CN103920627A (en) | 2014-04-29 | 2014-04-29 | Method for manufacturing polycrystal blowing crucibles for cast ingots |
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| CN103920627A true CN103920627A (en) | 2014-07-16 |
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| CN201410176566.XA Pending CN103920627A (en) | 2014-04-29 | 2014-04-29 | Method for manufacturing polycrystal blowing crucibles for cast ingots |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104609893A (en) * | 2015-01-30 | 2015-05-13 | 扬州荣德新能源科技有限公司 | Method of spraying silicon nitride on inner surface of efficient crucible |
| CN105063748A (en) * | 2015-08-14 | 2015-11-18 | 烟台核晶陶瓷新材料有限公司 | Efficient crucible for polycrystal ingot casting and preparation method of efficient crucible |
| CN105133011A (en) * | 2015-09-01 | 2015-12-09 | 晶科能源有限公司 | Polycrystalline quartz crucible coating and preparation method thereof |
| CN107185790A (en) * | 2017-05-15 | 2017-09-22 | 南通综艺新材料有限公司 | A kind of spraying coating process of G6 types high-efficiency polycrystalline blowing crucible |
| CN107739160A (en) * | 2017-11-15 | 2018-02-27 | 四川永祥硅材料有限公司 | A kind of spraying method of polycrystalline cast ingot crucible |
| CN108069731A (en) * | 2017-12-15 | 2018-05-25 | 江苏润弛太阳能材料科技有限公司 | A kind of casting polysilicon exempts to spray crucible silicon nitride coating and preparation method thereof |
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| JPS60197275A (en) * | 1984-03-19 | 1985-10-05 | Toyota Motor Corp | Water spray cooling method |
| CN101428273A (en) * | 2008-12-05 | 2009-05-13 | 江阴海润太阳能电力有限公司 | Silicon nitride spray finishing method for quartz crucible for polysilicon solar battery casting ingot |
| CN102040220A (en) * | 2009-10-13 | 2011-05-04 | 上海太阳能科技有限公司 | Manufacturing method of solar-grade polycrystalline silicon |
| CN102527594A (en) * | 2012-01-22 | 2012-07-04 | 常熟华融太阳能新型材料有限公司 | Quartz crucible for ingot casting and manufacturing method thereof |
| CN103361722A (en) * | 2013-07-23 | 2013-10-23 | 江西赛维Ldk太阳能高科技有限公司 | Polycrystalline silicon ingots and preparation method thereof, polycrystalline silicon chips and polycrystalline silicon ingot casting crucible |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS60197275A (en) * | 1984-03-19 | 1985-10-05 | Toyota Motor Corp | Water spray cooling method |
| CN101428273A (en) * | 2008-12-05 | 2009-05-13 | 江阴海润太阳能电力有限公司 | Silicon nitride spray finishing method for quartz crucible for polysilicon solar battery casting ingot |
| CN102040220A (en) * | 2009-10-13 | 2011-05-04 | 上海太阳能科技有限公司 | Manufacturing method of solar-grade polycrystalline silicon |
| CN102527594A (en) * | 2012-01-22 | 2012-07-04 | 常熟华融太阳能新型材料有限公司 | Quartz crucible for ingot casting and manufacturing method thereof |
| CN103361722A (en) * | 2013-07-23 | 2013-10-23 | 江西赛维Ldk太阳能高科技有限公司 | Polycrystalline silicon ingots and preparation method thereof, polycrystalline silicon chips and polycrystalline silicon ingot casting crucible |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104609893A (en) * | 2015-01-30 | 2015-05-13 | 扬州荣德新能源科技有限公司 | Method of spraying silicon nitride on inner surface of efficient crucible |
| CN105063748A (en) * | 2015-08-14 | 2015-11-18 | 烟台核晶陶瓷新材料有限公司 | Efficient crucible for polycrystal ingot casting and preparation method of efficient crucible |
| CN105063748B (en) * | 2015-08-14 | 2017-11-10 | 烟台核晶陶瓷新材料有限公司 | A kind of polycrystalline cast ingot high efficient crucible and preparation method thereof |
| CN105133011A (en) * | 2015-09-01 | 2015-12-09 | 晶科能源有限公司 | Polycrystalline quartz crucible coating and preparation method thereof |
| CN107185790A (en) * | 2017-05-15 | 2017-09-22 | 南通综艺新材料有限公司 | A kind of spraying coating process of G6 types high-efficiency polycrystalline blowing crucible |
| CN107739160A (en) * | 2017-11-15 | 2018-02-27 | 四川永祥硅材料有限公司 | A kind of spraying method of polycrystalline cast ingot crucible |
| CN108069731A (en) * | 2017-12-15 | 2018-05-25 | 江苏润弛太阳能材料科技有限公司 | A kind of casting polysilicon exempts to spray crucible silicon nitride coating and preparation method thereof |
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Application publication date: 20140716 |