CN103132141A - Coating composition of graphite equipment used for polycrystalline silicon ingot furnace - Google Patents
Coating composition of graphite equipment used for polycrystalline silicon ingot furnace Download PDFInfo
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- CN103132141A CN103132141A CN2011103978012A CN201110397801A CN103132141A CN 103132141 A CN103132141 A CN 103132141A CN 2011103978012 A CN2011103978012 A CN 2011103978012A CN 201110397801 A CN201110397801 A CN 201110397801A CN 103132141 A CN103132141 A CN 103132141A
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Abstract
The invention discloses a coating composition of graphite equipment used for a polycrystalline silicon ingot furnace. The coating composition of the graphite equipment used for the polycrystalline silicon ingot furnace is characterized by comprising, by weight, 5 to 30 percent of coating materials, 60 to 85 percent of solvent, wherein the coating materials are chosen from one type or a plurality types of silicon nitride, silicon carbide, silica and barium carbonate, and the solvent chosen from water or ethanol. The coating composition of the graphite equipment used for the polycrystalline silicon ingot furnace is capable of reducing carbon contamination of gasesous carbon silicon compound on polycrystalline silicon and preventing the graphite equipment from being damaged by silicon liquid while a crucible crazes and a pan is leaky.
Description
Technical field
The invention belongs to area of solar cell, be specifically related to for the coating composition of the graphite equipment of polycrystalline silicon ingot or purifying furnace, coating method and the purposes of this coating composition.
Background technology
In polycrystalline silicon ingot or purifying furnace, usually hold the silicon liquid of melting with quartz crucible, support quartz crucible under the condition of high temperature with the graphite backplate all around at quartz crucible, top is equipped with the graphite cover plate again and prevents that dust granules from falling in ingot, can also keep simultaneously thermal field stable, guarantee the quality of silicon ingot.
But under the condition of high temperature, graphite equipment surface has some graphite dusts and evaporates, can with the ingot casting process in some in the middle of gaseous substances, as reactions such as silicon monoxides, generate the silicide of carbon containing, make the carbon content in silicon ingot higher, affect the silicon ingot quality, and then can affect reliability and the work-ing life of solar cell device.
Occur sometimes simultaneously silicon hydrorrhea stream in the ingot casting process, this moment, silicon can be bonded on the graphite backplate firmly, made the damage of graphite equipment.
CN101812729A discloses polycrystal silicon ingot of a kind of low carbon content and preparation method thereof, has wherein mentioned apron internal surface coating silicon nitride or coat of silicon carbide composition at the graphite equipment.(content of mentioning silicon nitride in this coating composition or silicon carbide in [0089] section and [0090] section of the document is 80-100%.Being intended that with silicon nitride or silicon carbide of the document replaces the graphite backplate.
Summary of the invention
In view of above-mentioned mentioned problem, an object of the present invention is to provide a kind of coating composition of the graphite equipment for polycrystalline silicon ingot or purifying furnace, described coating composition contains:
Applicator 5-30wt%
Solvent 60-85wt%
Wherein said applicator is selected from one or more in silicon nitride, silicon carbide, silicon-dioxide and barium carbonate; Described solvent is selected from water or ethanol.
According to the present invention, the applicator that is used for this coating composition should be a kind of can be high temperature resistant, heat conductivility is good, the material lower with the wetting property of silicon, and therefore suitable applicator can comprise one or more mixtures of silicon nitride, silicon carbide, silicon-dioxide and barium carbonate etc.
According to of the present invention preferred embodiment a kind of, described ethanol can be dehydrated alcohol.
According to of the present invention preferred embodiment a kind of, be to guarantee compactness and the adhesivity of coat, preferred described coating substance is that granularity is approximately between the 0.1-100 micron, the particulate state of preferred 10-50 micron, and the thickness of final coating is between the 0.1-8 millimeter, and preferred thickness is the 1-3 millimeter.
According to of the present invention preferred embodiment a kind of, for further extending the work-ing life of this coating, can selectivity add appropriate additive in coating composition solution, comprise the binding agent that increases adhesive power, as silicon sol, polyvinyl alcohol etc.; With the dispersion agent that improves compactness, as amino alcohol etc.Wherein the content of dispersion agent can be 0.5-2wt%, and the content of binding agent can be 10-20wt%.
Can adopt method well known to those skilled in the art to prepare coating composition solution.For example, with above-mentioned material: applicator, as silicon nitride, silicon carbide, one or more in silicon-dioxide and barium carbonate and solvent are even, are mixed with coating composition solution.Can add according to actual needs dispersion agent and/or binding agent.
Second purpose of the present invention is to provide the coating method of described coating composition, it is characterized in that, carries out drying treatment after being coated in described coating composition on the graphite equipment.According to of the present invention one preferred embodiment, the coating composition solution for preparing can be used the mode of direct spraying or brushing to be coated on graphite equipment in ingot furnace, then carry out drying treatment, preferably carry out drying treatment under vacuum, vacuum tightness can be 10-100mbar, temperature can be 400-900 degree centigrade, and the time can be 4-10 hour.
The 3rd purpose of the present invention is to provide the purposes of described coating composition in applying the graphite equipment.
Graphite equipment of the present invention comprises graphite base plate (1), graphite cover plate (4), graphite backplate (3) and carbon fiber heat insulation cage body (5).Coating composition of the present invention can reduce the gaseous carbon silicon compound to the Prevent Carbon Contamination of polycrystal silicon ingot, and the while, also when crucible cracking colander, protection graphite equipment was avoided the damage of silicon liquid.
The present invention is used for the adjustment of coating composition by component concentration of the graphite equipment of polycrystalline silicon ingot or purifying furnace can be so that silicon nitride or silicon nitride coated layer and graphite base plate, backplate, and cover plate and carbon fiber heat insulation cage material have good bonding force.
Description of drawings
Embodiment
1, configuration coating composition solution: be the silicon nitride of 10 microns with 0.9 kilogram of particle diameter, the water of 2.1 kilograms mixes and obtains coating composition solution;
2, the mode of using spraying or brushing is coated in coating composition solution on graphite equipment in ingot furnace, and coat-thickness is 1 millimeter, then carries out vacuum drying treatment, and vacuum tightness is 15mbar, and temperature is 450 degrees centigrade, and the time is 5 hours.
3, with the graphite base plate of handling well, backplate, cover plate and carbon fiber heat insulation cage material are placed on the normal ingot casting of ingot furnace.
Embodiment 2
1, configuration coating composition solution: be the silicon nitride of 20 microns with 0.45 kilogram of particle diameter, the silicon sol of 0.45 kilogram, the water of 2.1 kilograms mix and obtain coating composition solution;
2, the mode of using spraying or brushing is coated in coating composition solution on graphite equipment in ingot furnace, and coat-thickness is 3 millimeters, then carries out vacuum drying treatment, and vacuum tightness is 50mbar, and temperature is 600 degrees centigrade, and the time is 6 hours.
3, with the graphite base plate of handling well, backplate, cover plate and carbon fiber heat insulation cage material are placed on the normal ingot casting of ingot furnace.
Embodiment 3
1, configuration coating composition solution: be the silicon nitride of 50 microns with 0.6 kilogram of particle diameter, the polyvinyl alcohol of 0.54 kilogram, the amino alcohol of 0.06 kilogram, the ethanol of 1.8 kilograms mix and obtain coating composition solution;
2, the mode of using spraying or brushing is coated in coating composition solution on graphite equipment in ingot furnace, and coat-thickness is 8 millimeters, then carries out vacuum drying treatment, and vacuum tightness is 100mbar, and temperature is 850 degrees centigrade, and the time is 10 hours.
3, with the graphite base plate of handling well, backplate, cover plate and carbon fiber heat insulation cage material are placed on the normal ingot casting of ingot furnace.
Embodiment 4
1, configuration coating composition solution: be the silicon carbide of 1 micron with 0.84 kilogram of particle diameter, the silicon sol of 0.3 kilogram, the amino alcohol of 0.06 kilogram, the water of 1.8 kilograms mix and obtain coating composition solution;
2, the mode of using spraying or brushing is coated in coating composition solution on graphite equipment in ingot furnace, and coat-thickness is 4 millimeters, then carries out vacuum drying treatment, and vacuum tightness is 50mbar, and temperature is 600 degrees centigrade, and the time is 6 hours.
3, with the graphite base plate of handling well, backplate, cover plate and carbon fiber heat insulation cage material are placed on the normal ingot casting of ingot furnace.
Embodiment 5
1, configuration coating composition solution: be the barium carbonate of 25 microns with 0.15 kilogram of particle diameter, the silicon sol of 0.3 kilogram, the amino alcohol of 0.03 kilogram, the water of 2.52 kilograms mix and obtain coating composition solution;
2, the mode of using spraying or brushing is coated in coating composition solution on graphite equipment in ingot furnace, and coat-thickness is 3 millimeters, then carries out vacuum drying treatment, and vacuum tightness is 80mbar, and temperature is 650 degrees centigrade, and the time is 7 hours.
3, with the graphite base plate of handling well, backplate, cover plate and carbon fiber heat insulation cage material are placed on the normal ingot casting of ingot furnace.
Embodiment 6
1, configuration coating composition solution: be the silicon-dioxide of 30 microns with 0.45 kilogram of particle diameter, the silicon sol of 0.45 kilogram, the amino alcohol of 0.06 kilogram, the water of 2.04 kilograms mix and obtain coating composition solution;
2, the mode of using spraying or brushing is coated in coating composition solution on graphite equipment in ingot furnace, and coat-thickness is 3 millimeters, then carries out vacuum drying treatment, and vacuum tightness is 80mbar, and temperature is 650 degrees centigrade, and the time is 7 hours.
3, with the graphite base plate of handling well, backplate, cover plate and carbon fiber heat insulation cage material are placed on the normal ingot casting of ingot furnace.
Embodiment 7
1, configuration coating composition solution: be the silicon nitride of 8 microns with 0.2 kilogram of particle diameter, 0.2 the kilogram particle diameter is the silicon carbide of 8 microns, 0.2 the kilogram particle diameter is the silicon-dioxide of 8 microns, 0.5 the silicon sol of kilogram, 0.06 the amino alcohol of kilogram, the water of 1.84 kilograms mixes and obtains coating composition solution;
2, the mode of using spraying or brushing is coated in coating composition solution on graphite equipment in ingot furnace, and coat-thickness is 3 millimeters, then carries out vacuum drying treatment, and vacuum tightness is 80mbar, and temperature is 650 degrees centigrade, and the time is 8 hours.
3, with the graphite base plate of handling well, backplate, cover plate and carbon fiber heat insulation cage material are placed on the normal ingot casting of ingot furnace.
Comparative Examples:
With the graphite base plate that is left intact, backplate, cover plate and carbon fiber heat insulation cage material are placed on the normal ingot casting of ingot furnace.
Claims (15)
1. be used for the coating composition of the graphite equipment of polycrystalline silicon ingot or purifying furnace, it is characterized in that, described coating composition contains:
Applicator 5-30wt%
Solvent 60-85wt%
Wherein said applicator is selected from one or more in silicon nitride, silicon carbide, silicon-dioxide and barium carbonate; Described solvent is selected from water or ethanol.
2. coating composition according to claim 1, is characterized in that, described ethanol is dehydrated alcohol.
3. coating composition according to claim 1 and 2, is characterized in that, described applicator is graininess.
4. coating composition according to claim 3, is characterized in that, the granularity of described particle is the 0.1-100 micron, is preferably the 10-50 micron.
5. according to claim 1-4 arbitrary described coating compositions, is characterized in that, the thickness of described coating composition is the 0.01-8 millimeter, is preferably the 1-3 millimeter.
6. according to claim 1-5 arbitrary described coating compositions, is characterized in that, described graphite equipment is graphite base plate (1), graphite cover plate (4), graphite backplate (3) and/or carbon fiber heat insulation cage body (5).
7. according to claim 1-6 arbitrary described coating compositions, is characterized in that, described coating composition also contains binding agent.
8. coating composition according to claim 7, is characterized in that, described binding agent is selected from silicon sol or polyvinyl alcohol.
9. according to claim 7 or 8 described coating compositions, is characterized in that, the content of described binding agent is 10-20wt%.
10. according to claim 1-9 arbitrary described coating compositions, is characterized in that, described coating composition also contains dispersion agent.
11. coating composition according to claim 10 is characterized in that, described dispersion agent is amino alcohol.
12. according to claim 10 or 11 described coating compositions is characterized in that, the content of described dispersion agent is 0.5-2wt%.
13. the coating method of according to claim 1-12 arbitrary described coating compositions is characterized in that, carries out drying treatment after being coated in described coating composition on the graphite equipment.
14. coating method according to claim 13 is characterized in that, described drying is to be that 10-100mbar, temperature are under the condition of 400-900 ℃ dry 4-10 hour in vacuum tightness.
15. the purposes of according to claim 1-12 arbitrary described coating compositions in applying the graphite equipment.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103526290A (en) * | 2013-10-24 | 2014-01-22 | 阿特斯(中国)投资有限公司 | Preparation method of polycrystalline silicon cast ingot |
| WO2014194832A1 (en) * | 2013-06-07 | 2014-12-11 | 英利能源（中国）有限公司 | Coating structure for crucible, fabrication method thereof, and crucible comprising same |
| CN104342752A (en) * | 2013-07-29 | 2015-02-11 | 晶科能源有限公司 | Method for ingoting polycrystalline silicon |
| CN104561963A (en) * | 2014-12-24 | 2015-04-29 | 无锡荣能半导体材料有限公司 | Method for preparing sintering-free coating of polycrystalline silicon ingot crucible |
| CN104562193A (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 |
| CN105112995A (en) * | 2015-08-19 | 2015-12-02 | 常州天合光能有限公司 | Compound separated carbon coating used for polysilicon ingot furnace, preparation method, graphite plate and polysilicon ingot furnace |
| CN105442042A (en) * | 2016-02-02 | 2016-03-30 | 江西赛维Ldk太阳能高科技有限公司 | Ingot furnace for reducing carbon content of polycrystalline silicon ingot and preparation method of ingot furnace |
| CN105568372A (en) * | 2015-12-30 | 2016-05-11 | 佛山市业丰赛尔陶瓷科技有限公司 | Coating composition for graphite equipment of polycrystalline silicon ingot furnace |
| CN105696070A (en) * | 2016-03-15 | 2016-06-22 | 常熟华融太阳能新型材料有限公司 | Novel graphite protective plate for polysilicon ingot casting and preparation method thereof |
| CN105803527A (en) * | 2016-05-23 | 2016-07-27 | 江苏协鑫硅材料科技发展有限公司 | Full fusion efficient polycrystalline silicon ingot casting method |
| CN108796617A (en) * | 2017-04-28 | 2018-11-13 | 友达晶材股份有限公司 | Crucible structure and manufacturing method thereof, and silicon crystal structure and manufacturing method thereof |
| CN110093664A (en) * | 2019-05-06 | 2019-08-06 | 新疆泰宇达环保科技有限公司 | A kind of polysilicon ingot mould and application method, preparation method for coating |
| CN110184650A (en) * | 2019-05-06 | 2019-08-30 | 新疆泰宇达环保科技有限公司 | Ingot mould coating and preparation method thereof for industrial silicon production |
| CN110719974A (en) * | 2017-04-27 | 2020-01-21 | 胜高股份有限公司 | Method for pulling up silicon single crystal |
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| CN101433890A (en) * | 2008-12-05 | 2009-05-20 | 江阴海润太阳能电力有限公司 | Method and device for spraying silicon nitride coating on inner wall of quartz crucible under low pressure |
| CN101812729A (en) * | 2010-04-28 | 2010-08-25 | 江西赛维Ldk太阳能高科技有限公司 | Polycrystalline silicon ingot with low carbon content and preparation method |
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Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014194832A1 (en) * | 2013-06-07 | 2014-12-11 | 英利能源（中国）有限公司 | Coating structure for crucible, fabrication method thereof, and crucible comprising same |
| CN104342752A (en) * | 2013-07-29 | 2015-02-11 | 晶科能源有限公司 | Method for ingoting polycrystalline silicon |
| CN103526290A (en) * | 2013-10-24 | 2014-01-22 | 阿特斯(中国)投资有限公司 | Preparation method of polycrystalline silicon cast ingot |
| CN104561963A (en) * | 2014-12-24 | 2015-04-29 | 无锡荣能半导体材料有限公司 | Method for preparing sintering-free coating of polycrystalline silicon ingot crucible |
| CN104562193B (en) * | 2015-01-30 | 2017-10-10 | 扬州荣德新能源科技有限公司 | A kind of casting method of polycrystal silicon ingot |
| CN104562193A (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 |
| CN105112995A (en) * | 2015-08-19 | 2015-12-02 | 常州天合光能有限公司 | Compound separated carbon coating used for polysilicon ingot furnace, preparation method, graphite plate and polysilicon ingot furnace |
| CN105568372A (en) * | 2015-12-30 | 2016-05-11 | 佛山市业丰赛尔陶瓷科技有限公司 | Coating composition for graphite equipment of polycrystalline silicon ingot furnace |
| CN105442042A (en) * | 2016-02-02 | 2016-03-30 | 江西赛维Ldk太阳能高科技有限公司 | Ingot furnace for reducing carbon content of polycrystalline silicon ingot and preparation method of ingot furnace |
| CN105442042B (en) * | 2016-02-02 | 2018-01-12 | 江西赛维Ldk太阳能高科技有限公司 | It is a kind of to be used to reduce ingot furnace of polycrystal silicon ingot carbon content and preparation method thereof |
| CN105696070A (en) * | 2016-03-15 | 2016-06-22 | 常熟华融太阳能新型材料有限公司 | Novel graphite protective plate for polysilicon ingot casting and preparation method thereof |
| CN105803527A (en) * | 2016-05-23 | 2016-07-27 | 江苏协鑫硅材料科技发展有限公司 | Full fusion efficient polycrystalline silicon ingot casting method |
| CN105803527B (en) * | 2016-05-23 | 2018-12-11 | 江苏协鑫硅材料科技发展有限公司 | A kind of method of fine melt efficient polycrystalline silicon ingot casting |
| CN110719974A (en) * | 2017-04-27 | 2020-01-21 | 胜高股份有限公司 | Method for pulling up silicon single crystal |
| CN110719974B (en) * | 2017-04-27 | 2021-09-07 | 胜高股份有限公司 | Method for pulling up silicon single crystal |
| CN108796617A (en) * | 2017-04-28 | 2018-11-13 | 友达晶材股份有限公司 | Crucible structure and manufacturing method thereof, and silicon crystal structure and manufacturing method thereof |
| CN110093664A (en) * | 2019-05-06 | 2019-08-06 | 新疆泰宇达环保科技有限公司 | A kind of polysilicon ingot mould and application method, preparation method for coating |
| CN110184650A (en) * | 2019-05-06 | 2019-08-30 | 新疆泰宇达环保科技有限公司 | Ingot mould coating and preparation method thereof for industrial silicon production |
| CN110184650B (en) * | 2019-05-06 | 2020-04-21 | 新疆泰宇达环保科技有限公司 | Ingot mold coating for industrial silicon production and preparation method thereof |
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Application publication date: 20130605 |