CN102417308A - Ingot casting quartz crucible silicon nitride coating sintering-free technology - Google Patents
Ingot casting quartz crucible silicon nitride coating sintering-free technology Download PDFInfo
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- CN102417308A CN102417308A CN2011102585637A CN201110258563A CN102417308A CN 102417308 A CN102417308 A CN 102417308A CN 2011102585637 A CN2011102585637 A CN 2011102585637A CN 201110258563 A CN201110258563 A CN 201110258563A CN 102417308 A CN102417308 A CN 102417308A
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Abstract
An ingot casting quartz crucible silicon nitride coating sintering-free technology comprises the following steps of: 1, raw material selection: selecting a silicon nitride powder, selecting water-soluble organic additives which contain one thousandth of 1-5 of a dispersant polyacrylic acid (PAA), one thousandth of 3-5 of a binder polyvinyl alcohol (PVA) and one thousandth of 3-6 of a moisture-proof agent glue 107, selecting 1000-1300ml/per unit of a solution pure water; 2, material preparation: weighing the silicon nitride powder and the binder polyvinyl alcohol (PVA) at one thousandth of 3-5 and dissolving by pure water, weighing the dispersant polyacrylic acid (PAA) at one thousandth of 1-5 and weighing the glue 107 at one thousandth of 3-6; 3, preparation; and 4, spraying. The technology provided by the invention is used to simplify the process, reduce cost, shorten the period of the crucible coating production, prolong the service life of quartz crucible and enhance security. In addition, by the adoption of the technology, silicon ingot has high utilization rate and good quality.
Description
Technical field
The present invention relates to a kind of ingot casting with the unburned technology of quartz crucible silicon nitride coating.
Background technology
Polycrystalline silicon ingot casting prepares in the process, and high-purity silica pot is its indispensable container, can prepare the fine polycrystal silicon ingot because of its purity is high.In the polycrystalline silicon ingot casting process, in the fusing of silicon material, crystal growth, annealing refrigerative process, single use high-purity silica pot will face following harm:
(1) work-ing life short, poor stability: when silicon melt and quartz crucible Long contact time, can produce glutinousness, Si and SiO
2Reaction generates SiO and makes and crucible attenuation even cracking cause heavy losses such as silicon hydrorrhea stream, reduces work-ing life, poor stability.
(2) the silicon ingot utilization ratio is low: crucible and silicon liquid produce viscid; In the silicon ingot process of cooling; Cause breaking of crucible and silicon ingot owing to both thermal expansivity are different; Cause the rate variance that utilizes of silicon ingot, simultaneously available silico briquette maybe the silicon chip fragmentation rate increases in the slicing processes owing to unrelieved stress causes greatly.
(3) pollute silicon ingot: the raw material that ingot casting uses is the HIGH-PURITY SILICON material of Si content up to 99.9999% (6N); And the purity of high-purity silica pot is more than 99.7; Directly use quartz crucible will cause a large amount of impurity to get into the silicon ingot from crucible; Like C, O, Fe, B, P etc., pollute silicon ingot, the electricity of change silicon ingot, mechanical property etc.
Therefore, the problems referred to above that occur in order to solve direct use crucible are utilized Si usually on technological measure
3N
4Material becomes coating, be sprayed on the inwall of quartz crucible after, sintering at high temperature, coating and crucible are integrally formed, thereby have isolated contacting of silicon melt and quartz crucible; It not only can solve viscid problem, and can reduce impurity concentrations such as C in the polysilicon, O, Fe, B, P; Utilize Si in addition
3N
4Coating, the ingot casting security that can also improve quartz crucible reaches the purpose that reduces production costs.
After the silicon nitride coating spraying is good, combine with quartz crucible closely, crucible is put into the drawer kiln in order to make silicon nitride coating; Roasting is to about 1050-1100 ℃; Through the roasting of 21h, discharge the planar water in crucible and the silicon nitride coating, make between coating and the crucible better to combine.Yet because performance there are differences between silicon nitride slurry and the quartz crucible, both associativities are relatively poor, after crucible spraying and the roasting, occur big area dry linting and skin effect phenomenon easily, cause spraying effect to reduce.In addition, quartz crucible is in roasting process, and the bad crystallization that just is easy to of temperature control causes the heat-shock resistance of crucible to descend, and in process of cooling, produces the be full of cracks defective thereby bring out quartz crucible, causes in the ingot casting process, taking place the siliconising phenomenon.
Summary of the invention
Its purpose of the present invention just is to provide a kind of ingot casting with the unburned technology of quartz crucible silicon nitride coating; Not only simplify operation, but also reduced cost, shortened the crucible coating layer production cycle; Have long service life, characteristics that security is good, and the silicon ingot utilization ratio is high, the silicon ingot quality is good.
The technical scheme that realizes above-mentioned purpose and take comprises
1) material choice:
1.1 silicon nitride powder is selected, silicon nitride powder;
1.2 water-soluble organic additive is selected
Dispersion agent is selected: ROHM (PAA) dispersion agent, consumption 1-5 ‰;
Sticker is selected: Z 150PH (PVA) sticker, consumption 3-5 ‰;
Non-blushing thinner is selected: 107 glue, consumption 3-6 ‰;
1.3 solution is selected: pure water, consumption 1000-1300ml/;
2) get the raw materials ready: silicon nitride powder, Z 150PH (PVA) sticker are in 3-5 ‰ ratio weighing, with pure water dissolving earlier; ROHM PAA dispersion agent is in 1-5 ‰ ratio weighing; 107 glue are in 3-6 ‰ ratio weighing;
3) preparation: ROHM PAA raw material that weighs up and 107 glue are poured in the PVAC polyvinylalcohol solution cup, stirred; Add the 1300ml pure water then, after stirring once more, silicon nitride powder is poured into, stir, sealing just can be used after placing 100min;
4) spraying, whole silicon nitride slurries that will prepare with spray gun evenly are sprayed on body temperature on 50-70 ℃ inner wall of quartz crucible and bottom, dry 1-3h under 50-70 ℃ temperature, but cooling is used with regard to ingot casting after placing 100min.
Compared with prior art; Beneficial effect of the present invention is, owing to adopted the unburned process method of silicon nitride coating, thereby not only simplified operation; But also reduced cost; Shortened the crucible coating layer production cycle, had long service life, characteristics that security is good, and the silicon ingot utilization ratio is high, the silicon ingot quality is good.
Embodiment
Comprise
1) material choice:
1.1 silicon nitride powder is selected, silicon nitride powder;
1.2 water-soluble organic additive is selected
Dispersion agent is selected: ROHM (PAA) dispersion agent, consumption 1-5 ‰;
Sticker is selected: Z 150PH (PVA) sticker, consumption 3-5 ‰;
Non-blushing thinner is selected: 107 glue, consumption 3-6 ‰;
1.3 solution is selected: pure water, consumption 1000-1300ml/;
2) get the raw materials ready: silicon nitride powder, Z 150PH (PVA) sticker are in 3-5 ‰ ratio weighing, with pure water dissolving earlier; ROHM PAA dispersion agent is in 1-5 ‰ ratio weighing; 107 glue are in 3-6 ‰ ratio weighing;
3) preparation: ROHM PAA raw material that weighs up and 107 glue are poured in the PVAC polyvinylalcohol solution cup, stirred; Add the 1300ml pure water then, after stirring once more, silicon nitride powder is poured into, stir, sealing just can be used after placing 100min;
4) spraying, whole silicon nitride slurries that will prepare with spray gun evenly are sprayed on body temperature on 50-70 ℃ inner wall of quartz crucible and bottom, dry 1-3h under 50-70 ℃ temperature, but cooling is used with regard to ingot casting after placing 100min.
Described silicon nitride powder is chosen Japanese UBE company's silicon nitride powder and German H.C Starck company silicon nitride powder, mixes and uses, and each quartz crucible is individual with 400-500g/.
In order to ensure the crucible coating quality; Avoid coating be full of cracks because of causing in the sintering process; Influence the silicon ingot quality, the unburned knot technology of this crucible coating layer is promptly added the element such as dispersion agent, sticker, non-blushing thinner of the water soluble organic substance macromolecule material of 3-5 ‰ wt in the silicon nitride slurry; Through organic macromolecule chemisorption and the big physisorption of silicon nitride powder specific surface area, make silicon nitride powder effectively be adsorbed on the crucible inwall.Wherein, the effect of dispersion agent is that alpha-silicon nitride powders is spread out in water solvent, makes the rheological characteristics of slurry stable; Adding the sticker purpose is to improve the viscosity of silicon nitride slurry, the silicon nitride powder that is sprayed in the quartz crucible is adsorbed on the crucible inwall forcefully through high molecular chemisorption, thereby is difficult for dry linting; Non-blushing thinner can prevent effectively that airborne water molecules from getting in the silicon nitride coating because water tolerance is better, thereby avoids silicon nitride powder to come off because of wet swelling causes cracking.The a small amount of organism that adds will or be cracked into carbon with the molecular form volatilization before 1410 ℃ in the ingot casting process; Because the temperature vibration property of carbon is bigger; Add to vacuumize in the ingot furnace and the air-flow convection action that carbon will volatilize, organic adding can not produce bigger influence to the quality of crystal ingot.Therefore, the present invention compares with traditional technology, has not only simplified operation, but also has reduced cost, has shortened the crucible coating layer production cycle.Specific practice is:
1) material choice:
1.1 silicon nitride powder is selected: choose Japanese UBE company's silicon nitride powder and German H.C Starck company silicon nitride powder, mix and use, each quartz crucible is individual with 400-500g/;
1.2 water-soluble organic additive is selected
Dispersion agent is selected: ROHM (PAA) dispersion agent, consumption 1-5 ‰;
Sticker is selected: Z 150PH (PVA) sticker, consumption 3-5 ‰;
Non-blushing thinner is selected: 107 glue, consumption 3-6 ‰;
1.3 solution is selected: pure water, consumption 1000-1300ml/;
2) get the raw materials ready: silicon nitride powder 450g; Z 150PH (PVA) sticker is in 3-5 ‰ ratio weighing 3g, with pure water dissolving earlier; ROHM (PAA) dispersion agent is in 1-5 ‰ ratio weighing 2.5g; 107 glue are in 3-6 ‰ ratio weighing 2.6g;
3) preparation: PAA raw material that weighs up and 107 glue are poured in the PVA solution cup, stirred; Add the 1300ml pure water then, after stirring once more, the 450g silicon nitride powder is poured into, stir, sealing just can be used after placing 100min;
Whole silicon nitride slurries that will prepare with spray gun evenly are sprayed on body temperature on 50-70 ℃ inner wall of quartz crucible and bottom, dry 1-3h under 50-70 ℃ temperature, but cooling is used with regard to ingot casting after placing 100min.
Usually the quartz crucible that has sprayed silicon nitride coating needs the roasting of process 21h under 1050-1100 ℃ of left and right sides temperature, and it is very big to consume energy.Adopt the present invention just to save mass energy; And can save the spending of buying sintering oven.
Embodiment
With ingot casting 450kg polycrystal silicon ingot is example:
Choice of equipment: select the GT450 ingot furnace for use, and to be of a size of 878 * 878 * 480mm quartz crucible be charge cask.Crucible is placed on preheating on the square rotative heater through after the assay was approved, and preheating temperature is 50-70 ℃.
Embodiment 1:
Get the raw materials ready: silicon nitride powder 450g; Vltra tears sticker (HPMC) 3.1g is with pure water dissolving earlier; Thanomin dispersion agent 2.5g; 107 glue 2.6g;
Preparation: thanomin raw material that weighs up and 107 glue are poured in the Gonak cup, stirred; Add the 1300ml pure water then, after stirring once more, the 450g silicon nitride powder is poured into, stir, sealing just can be used after placing 100min;
Whole silicon nitride slurries that will prepare with spray gun evenly are sprayed on body temperature on 50-70 ℃ inner wall of quartz crucible and bottom, dry 1-3h under 50-70 ℃ temperature, but cooling is used with regard to ingot casting after placing 100min.
Embodiment 2
Get the raw materials ready: silicon nitride powder 450g; Emulsion binder 3.5g is with pure water dissolving earlier; ROHM (PAA) dispersion agent 2.3g; 107 glue 2.4g;
Preparation: PAA raw material that weighs up and 107 glue are poured in the latex solution cup, stirred; Add the 1300ml pure water then, after stirring once more, the 450g silicon nitride powder is poured into, stir, sealing just can be used after placing 100min;
Whole silicon nitride slurries that will prepare with spray gun evenly are sprayed on body temperature on 50-70 ℃ inner wall of quartz crucible and bottom, dry 1-3h under 50-70 ℃ temperature, but cooling is used with regard to ingot casting after placing 100min.
Claims (2)
1. an ingot casting is characterized in that with the unburned technology of quartz crucible silicon nitride coating, comprises
1) material choice:
1.1 silicon nitride powder is selected, silicon nitride powder;
1.2 water-soluble organic additive is selected
Dispersion agent is selected: ROHM (PAA) dispersion agent, consumption 1-5 ‰;
Sticker is selected: Z 150PH (PVA) sticker, consumption 3-5 ‰;
Non-blushing thinner is selected: 107 glue, consumption 3-6 ‰;
1.3 solution is selected: pure water, consumption 1000-1300ml/;
2) get the raw materials ready: silicon nitride powder, Z 150PH (PVA) sticker are in 3-5 ‰ ratio weighing, with pure water dissolving earlier; ROHM PAA dispersion agent is in 1-5 ‰ ratio weighing; 107 glue are in 3-6 ‰ ratio weighing;
3) preparation: ROHM PAA raw material that weighs up and 107 glue are poured in the PVAC polyvinylalcohol solution cup, stirred; Add the 1300ml pure water then, after stirring once more, silicon nitride powder is poured into, stir, sealing just can be used after placing 100min;
4) spraying, whole silicon nitride slurries that will prepare with spray gun evenly are sprayed on body temperature on 50-70 ℃ inner wall of quartz crucible and bottom, dry 1-3h under 50-70 ℃ temperature, but cooling is used with regard to ingot casting after placing 100min.
2. the described a kind of ingot casting of root a tree name claim 1 is with the unburned technology of quartz crucible silicon nitride coating; It is characterized in that; Described silicon nitride powder is chosen Japanese UBE company's silicon nitride powder and German H.C Starck company silicon nitride powder, mixes and uses, and each quartz crucible is individual with 400-500g/.
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| CN2011102585637A CN102417308A (en) | 2011-09-03 | 2011-09-03 | Ingot casting quartz crucible silicon nitride coating sintering-free technology |
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| CN2011102585637A CN102417308A (en) | 2011-09-03 | 2011-09-03 | Ingot casting quartz crucible silicon nitride coating sintering-free technology |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102797042A (en) * | 2012-09-06 | 2012-11-28 | 张礼强 | Crucible for melting crystalline silicon, method for producing crucible and spray coating liquid |
| 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 |
| CN102898034A (en) * | 2012-09-28 | 2013-01-30 | 东海晶澳太阳能科技有限公司 | Preparation method of crucible silicon nitride coating for crystalline silicon cast ingot |
| CN103663998A (en) * | 2012-09-17 | 2014-03-26 | 无锡尚德太阳能电力有限公司 | Preparation method of internal coating of crucible for crystalline silicon ingots |
| CN107312432A (en) * | 2017-06-23 | 2017-11-03 | 石家庄优士科电子科技有限公司 | Polycrystalline silicon ingot casting silica crucible silicon nitride coating binding agent and preparation method thereof |
| CN107916451A (en) * | 2017-12-15 | 2018-04-17 | 江苏润弛太阳能材料科技有限公司 | One kind casting polysilicon exempts to spray crucible |
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| CN101508590A (en) * | 2009-03-20 | 2009-08-19 | 江西赛维Ldk太阳能高科技有限公司 | Crucible pot coating for polysilicon casting ingot and preparation method |
| CN101844935A (en) * | 2010-05-31 | 2010-09-29 | 江西赛维Ldk太阳能高科技有限公司 | Crucible coating layer for polycrystal silicon or single crystal silicon and preparation method thereof |
| US20110014582A1 (en) * | 2009-07-16 | 2011-01-20 | Memc Singapore Pte. Ltd. (Uen200614794D) | Coated crucibles and methods for applying a coating to a crucible |
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| CN101508590A (en) * | 2009-03-20 | 2009-08-19 | 江西赛维Ldk太阳能高科技有限公司 | Crucible pot coating for polysilicon casting ingot and preparation method |
| US20110014582A1 (en) * | 2009-07-16 | 2011-01-20 | Memc Singapore Pte. Ltd. (Uen200614794D) | Coated crucibles and methods for applying a coating to a crucible |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102797042A (en) * | 2012-09-06 | 2012-11-28 | 张礼强 | Crucible for melting crystalline silicon, method for producing crucible and spray coating liquid |
| WO2014036864A1 (en) * | 2012-09-06 | 2014-03-13 | Zhang Liqiang | Crucible for melting crystalline silicon, method for producing crucible and spray coating liquid |
| CN102797042B (en) * | 2012-09-06 | 2015-06-10 | 张礼强 | Crucible for melting crystalline silicon, method for producing crucible and spray coating liquid |
| CN103663998A (en) * | 2012-09-17 | 2014-03-26 | 无锡尚德太阳能电力有限公司 | Preparation method of internal coating of crucible for crystalline silicon ingots |
| 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 |
| CN102898034A (en) * | 2012-09-28 | 2013-01-30 | 东海晶澳太阳能科技有限公司 | Preparation method of crucible silicon nitride coating for crystalline silicon cast ingot |
| CN102898034B (en) * | 2012-09-28 | 2015-02-18 | 东海晶澳太阳能科技有限公司 | Preparation method of crucible silicon nitride coating for crystalline silicon cast ingot |
| CN107312432A (en) * | 2017-06-23 | 2017-11-03 | 石家庄优士科电子科技有限公司 | Polycrystalline silicon ingot casting silica crucible silicon nitride coating binding agent and preparation method thereof |
| CN107312432B (en) * | 2017-06-23 | 2019-09-03 | 石家庄优士科电子科技有限公司 | Polycrystalline silicon ingot casting silica crucible silicon nitride coating binder and preparation method thereof |
| CN107916451A (en) * | 2017-12-15 | 2018-04-17 | 江苏润弛太阳能材料科技有限公司 | One kind casting polysilicon exempts to spray crucible |
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Application publication date: 20120418 |