CN102719889A - Polysilicon ingot casting process - Google Patents
Polysilicon ingot casting process Download PDFInfo
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- CN102719889A CN102719889A CN2012102239427A CN201210223942A CN102719889A CN 102719889 A CN102719889 A CN 102719889A CN 2012102239427 A CN2012102239427 A CN 2012102239427A CN 201210223942 A CN201210223942 A CN 201210223942A CN 102719889 A CN102719889 A CN 102719889A
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Abstract
The invention discloses a polysilicon ingot casting process. The process comprises the following steps of: dehydrating a crucible on which a silicon nitride coating is sprayed, filling a polysilicon material, and putting into an ingot furnace; raising the temperature of the ingot furnace to a sintering temperature within a preset time range, and maintaining the sintering temperature for a preset time to ensure that the silicon nitride coating can be conveniently sintered on the inner wall of the crucible; and finally, adjusting a temperature in the ingot furnace from the sintering temperature to a polysilicon material fusion temperature, a crystal growth temperature, an annealing temperature and a cooling temperature sequentially, and performing a polysilicon fusion process, a crystal growth process, an annealing process and a cooling process at corresponding temperatures respectively. By the process, the silicon nitride coating of the crucible can be sintered by adjusting the temperature of an ingot casting process, so that the economization of equipment cost and labor cost is facilitated, and the processing efficiency of a polysilicon ingot can be improved; and the sintered silicon nitride coating has a good isolation effect on quartz ceramics and the polysilicon material, and polysilicon ingots with high quality can be prepared.
Description
Technical field
The present invention relates to the polycrystalline silicon ingot casting technical field, particularly a kind of polycrystalline silicon casting ingot process.
Background technology
Photovoltaic solar is used the polycrystalline silicon ingot casting field; When casting polycrystalline silicon, use quartz ceramic crucible to carry mould as the silicon material; High-purity polycrystalline silicon raw material is contained in the crucible of band silicon nitride coating; Through in ingot furnace internal heating, fusing, crystallographic orientation, annealing, five technological processs of cooling, finally make the high purity polycrystalline silicon material grow into the polycrystal silicon ingot that is used to produce used for solar batteries.
The purpose of inner surface of crucible coating silicon nitride mainly be protection quartz crucible (staple is a silicon-dioxide) at high temperature with the isolation of silicon; Stop silicon-dioxide and the reaction of silicon liquid in the casting ingot process; Prevent to pollute HIGH-PURITY SILICON liquid; Guarantee simultaneously after the crystallization of silicon liquid not and the crucible phenomenon that sticks together,, guarantee silicon ingot demoulding integrity so that polycrystal silicon ingot is after quartz crucible breaks and cools off.
At present, the polycrystalline silicon ingot casting field mainly adopts two kinds of methods to realize effectively adhering to of crucible top layer silicon nitride coating, and first method is the high temperature sintering method; This method mainly stirs alpha-silicon nitride powders and pure water by a certain percentage, and stir back spraying or brushing are at crucible surface, under the condition of heating; Make silicon nitride solution be adsorbed on inner surface of crucible uniformly; Form the powdery coating, then the crucible of band coating is carried out high temperature and bake, make the silicon nitride firm attachment in crucible surface.
Second method is for adding certain additive when spraying silicon nitride; That is: in the mixing solutions of alpha-silicon nitride powders and pure water, use additive; The effect of additive is to producing the adhesion effect between the alpha-silicon nitride powders and between alpha-silicon nitride powders and the inner surface of crucible; Make silicon nitride coating solidify at crucible surface rapidly, thereby remove the high bake step of coating from.
From above-mentioned two kinds of method service conditions, the high temperature sintering method is comparatively complicated, needs independently agglomerating plant, and energy consumption and cost are higher; Additive method has been introduced new impurity concerning HIGH-PURITY SILICON liquid; Pollute silicon liquid; Reduce the quality of silicon ingot fringe region, just silicon nitride particle is had the adhesion effect, additives decompose under the high temperature because of additive simultaneously; Silicon nitride coating intensity and compactness can't realize provide protection, and the polycrystalline silicon ingot casting stably manufactured is brought very big hidden danger.
Therefore, how a kind of energy of both having saved being provided, can guaranteeing the technology of silicon nitride coating sintering quality on the crucible again, is the technical problem that those skilled in that art need to be resolved hurrily.
Summary of the invention
The object of the invention is accomplished the sintering to crucible coating layer for a kind of polycrystalline silicon casting ingot process is provided in this technology, realized on the basis that guarantees the silicon nitride coating sintering quality, saving the target of the energy.
For solving the problems of the technologies described above, the present invention provides a kind of polycrystalline silicon casting ingot process, and this technological process may further comprise the steps:
S1, will scribble the crucible dehydration of silicon nitride coating after, the splendid attire polycrystalline silicon material also places ingot furnace;
S2, the temperature with ingot furnace in the Preset Time scope rise to sintering temperature, and keep the said sintering temperature scheduled time so that said silicon nitride coating is sintered on the inwall of said crucible;
S3, the temperature in the ingot furnace is adjusted to said polycrystalline silicon material temperature of fusion, long brilliant temperature, annealing temperature, cooling temperature by sintering temperature successively, under relevant temperature, accomplishes the fusing of polysilicon, long crystalline substance, annealing, process for cooling respectively.
Preferably, in said step S2, the scheduled time scope of keeping said sintering temperature is 45min-120min.
Preferably, in said step S3, the time range that said sintering temperature is adjusted to said polycrystalline silicon material temperature of fusion is 300min～370min.
Preferably, in said step S2, it is 0min～130min that said Preset Time is chosen scope.
Preferably, said sintering range is 800 ℃-1100 ℃.
Preferably, in said step S1, the spraying coating process TR of said silicon nitride coating is 50 ℃-100 ℃.
Preferably, before said step S1, also have following steps:
S0, outfit silicon nitride solution, the ratio range of silicon nitride and pure water is in the said silicon nitride solution: 0.2g/ml～0.27g/ml.
Preferably, in said step S1, place air 0.5h～2h realization dehydration or place drying oven to realize dehydration through the crucible after will spraying.
In the polycrystalline silicon casting ingot process provided by the present invention; With directly carrying out the splendid attire polycrystalline silicon material after the crucible dehydration that is coated with silicon nitride; Temperature through regulating the casting ingot process ingot furnace is accomplished the sintering to the silicon nitride coating of crucible; And after accomplishing the silicon nitride coating sintering, continue to regulate the preparation that the ingot furnace temperature is finally accomplished polycrystal silicon ingot; Compared with prior art; The present invention utilizes the temperature of regulating casting ingot process, accomplishes the silicon nitride coating sintering of crucible, can save the equipment that is provided with for special sintered silicon nitride coating in the prior art; Help saving equipment cost, cost of labor; And the silicon nitride coating agglomerating process of crucible, splendid attire absorbs heat simultaneously in the inner polycrystalline silicon material of crucible, can improve the working (machining) efficiency of polycrystal silicon ingot.
And the silicon nitride coating that sintering is accomplished stands higher temperature again and also can play the good isolation effect to quartz-ceramics and polycrystalline silicon material, guarantees normally carrying out of polycrystalline silicon casting ingot process, the polycrystal silicon ingot that preparation has better quality.
Description of drawings
Fig. 1 is the schema of polycrystalline silicon casting ingot process provided by the present invention.
Embodiment
Core of the present invention is accomplished the sintering to crucible coating layer for a kind of polycrystalline silicon casting ingot process is provided in this technology, realized on the basis that guarantees the silicon nitride coating sintering quality, saving the target of the energy.
In order to make those skilled in the art understand technical scheme of the present invention better, the present invention is done further detailed description below in conjunction with accompanying drawing and specific embodiment.
Please refer to Fig. 1, Fig. 1 is the schema of polycrystalline silicon casting ingot process provided by the present invention.
The invention provides a kind of polycrystalline silicon casting ingot process, this technological process may further comprise the steps:
S1, will scribble the crucible dehydration of silicon nitride coating after, the splendid attire polycrystalline silicon material also places ingot furnace;
Crucible described in this paper mainly is meant with the quartz-ceramics material and as the crucible body vessel that one deck has the silicon nitride material coating of suitable thickness is set evenly on the inwall of quartz-ceramics material.General at first the mode of silicon nitride coating through spraying or brushing; The solution spraying that will contain silicon nitride is in the inwall of crucible body; Wherein silicon nitride solution can be prepared by following mode: at first prepare a certain amount of ground in advance alpha-silicon nitride powders, an amount of pure water stirring at low speed; Secondly stirring at low speed pure water is poured in the pure water that is stirring with the casserole alpha-silicon nitride powders with ground slowly then, treats that silicon nitride all puts in the pure water; Begin to spray to the crucible inwall behind the high-speed stirring 10min, finish up to the whole sprayings of all silicon nitride solution.
After the crucible that spraying is finished places air to place 0.5h～2h its silicon nitride layer is dewatered fully, again with the polycrystalline silicon material splendid attire in crucible, the crucible with charging is positioned in the ingot furnace then.Silicon nitride coating after the dehydration is difficult for being damaged in splendid attire polycrystalline silicon material process, guarantees in the follow-up sintering process, to form complete sinter fuse coating.
S2, the temperature with ingot furnace in the Preset Time scope rise to sintering temperature, and keep the said sintering temperature scheduled time so that said silicon nitride coating is sintered on the inwall of said crucible;
In this step according to the difference of the set heating installation power of different ingot furnaces; Can be chosen in the interior temperature of different Preset Time scopes and rise to silicon nitride coating agglomerating sintering temperature ingot furnace; This sintering temperature is lower than the temperature of fusion of polycrystalline silicon material; When temperature maintenance in the ingot furnace in this sintering temperature after the scheduled time, silicon nitride coating can tight burning in the crucible inwall; Sintering temperature can be selected the desired value in 800 ℃～1100 ℃ scopes in this step.
Keeping the scheduled time of sintering temperature can take all factors into consideration the situation such as watt level of sintering quality, use properties and the ingot furnace of power consumption, silicon nitride coating and confirm according to practical experience.
S3, the temperature in the ingot furnace is adjusted to said polycrystalline silicon material temperature of fusion, long brilliant temperature, annealing temperature, cooling temperature by sintering temperature successively, under relevant temperature, accomplishes the fusing of polysilicon, long crystalline substance, annealing, process for cooling respectively.
As step S2) in the silicon nitride coating sintering finish after; Temperature in the ingot furnace is risen to the temperature of fusion of polycrystalline silicon material; Make the polycrystalline silicon material solid of splendid attire in the crucible slowly be molten into liquid silicon, until fusing fully, usually; According to the difference of ingot furnace plant capacity, this melting process needs about 240min～260min.
After polycrystalline silicon material was molten into liquid silicon fully, the temperature of regulating in the ingot furnace made it reach the required brilliant temperature of length of long brilliant technology, accomplishes the liquid silicon recrystallize, forms polycrystal silicon ingot; This process approximately needs 1300min～1700min.
After long brilliant technology finishes, slowly reduce temperature in the ingot furnace so that eliminate the polycrystal silicon ingot internal stress, this technology becomes annealing process, and accomplishing this technology approximately needs 60min～120min.
Be the process for cooling step at last, promptly polycrystal silicon ingot lowered the temperature, the temperature in the ingot furnace is reduced to about 450 ℃, polycrystal silicon ingot is taken out from ingot furnace.
In the polycrystalline silicon casting ingot process provided by the present invention; With directly carrying out the splendid attire polycrystalline silicon material after the crucible dehydration that is coated with silicon nitride; Temperature through regulating the casting ingot process ingot furnace is accomplished the sintering to the silicon nitride coating of crucible; And after accomplishing the silicon nitride coating sintering, continue to regulate the preparation that the ingot furnace temperature is finally accomplished polycrystal silicon ingot; Compared with prior art; The present invention utilizes the temperature of regulating casting ingot process, accomplishes the silicon nitride coating sintering of crucible, can save the equipment that is provided with for special sintered silicon nitride coating in the prior art; Help saving equipment cost, cost of labor; And the silicon nitride coating agglomerating process of crucible, splendid attire absorbs heat simultaneously in the inner polycrystalline silicon material of crucible, can improve the working (machining) efficiency of polycrystal silicon ingot.
And the silicon nitride coating that sintering is accomplished stands higher temperature again and also can play the good isolation effect to quartz-ceramics and polycrystalline silicon material, guarantees normally carrying out of polycrystalline silicon casting ingot process, the polycrystal silicon ingot that preparation has better quality.
Evidence, the appearance quality behind the silicon nitride coating sintering is relevant with the time, and sintering time is short more, and the visual appearance of silicon nitride coating is poor more, and when sintering time was lower than 45min, the visual appearance behind the silicon nitride coating sintering was poor; But also be not to mean, sintering time is long more, and the sintered surface quality of silicon nitride coating is good more, facts have proved, and after sintering time surpasses certain hour, not bigger variation of the surface quality of silicon nitride coating behind the sintering.
Therefore, a kind of preferred embodiment in, at above-mentioned steps S2) in; The scheduled time scope of keeping said sintering temperature is 45min-120min, and this time range can satisfy the sintering requirement of existing different capacity ingot furnace equipment to the silicon nitride coating of crucible, both can guarantee the surperficial sintering visual appearance of silicon nitride coating; Satisfy the request for utilization of casting ingot process; Guarantee the quality of production of polycrystal silicon ingot, can save silicon nitride coating agglomerating energy consumption again, cut down finished cost.
Certainly, also can pass through test of many times, obtain the scheduled time of the best sintered silicon nitride coating of this ingot furnace to the ingot furnace of a certain concrete power.
Step S3 at above-mentioned each embodiment) in; The time range that sintering temperature is adjusted to said polycrystalline silicon material temperature of fusion is 300min～370min; The temperature of fusion of polycrystalline silicon material is generally 1500 ℃～1560 ℃, that is to say, at 300min～in the time of the 370min left and right sides; Temperature in the ingot furnace from 800 ℃～1100 ℃ of the sintering temperatures of silicon nitride coating, is increased to 1500 ℃～1560 ℃.
In this embodiment; Sintering temperature is adjusted to the choosing of time range of said polycrystalline silicon material temperature of fusion and has not only satisfied the sintering demand of existing stage different capacity ingot furnace to silicon nitride coating; And in this time range, reaching the temperature of fusion of polysilicon, minimizing that can be as far as possible little is to the influence of silicon nitride coating visual appearance.
Step S2 at above-mentioned each embodiment) in, the scope of Preset Time can be made as any number of 0min～130min, and confirming of this concrete numerical value can be by concrete ingot furnace decision.
Sintering range among above-mentioned each embodiment can be 800 ℃～1100 ℃, and Temperature numerical can satisfy the sintering of silicon nitride coating basically in this scope, and equipment energy consumption is lower; Certainly, the numerical value of sintering temperature also not exclusively is confined to the said temperature scope, as long as can accomplish the sintering of silicon nitride coating, and is lower than the polycrystalline silicon material temperature of fusion and gets final product.
Among above-mentioned each embodiment, step S1) the spraying coating process TR of silicon nitride coating can be 50 ℃～100 ℃ described in, and this TR helps forming coating thickness silicon nitride coating relatively uniformly.
Among above-mentioned each embodiment, at said step S1) precedingly can also increase following steps:
S0, outfit silicon nitride solution, the ratio range of silicon nitride and pure water is in the said silicon nitride solution: 0.2～0.27g/ml;
The coating thickness of silicon nitride coating can be 1mm～2mm, and the silicon nitride solution of preparation can satisfy the demand of different coating thickness basically in this ratio range; For example in a kind of embodiment, can choose alpha-silicon nitride powders 350g～400g and stir and in pure water 1500ml～1800ml, be mixed with emulsion state silicon nitride solution.
At said step S1) in, the dewatering type of spraying back silicon nitride coating can be placed in the drying oven by various ways, realizes fast dewatering; Also can place air 0.5h～2h to realize dehydration through the crucible after will spraying, place the air dewatering type to need not to consume the extra energy, save cost.
More than a kind of polycrystalline silicon casting ingot process provided by the present invention has been carried out detailed introduction.Used concrete example among this paper principle of the present invention and embodiment are set forth, the explanation of above embodiment just is used for helping to understand method of the present invention and core concept thereof.Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of claim of the present invention.
Claims (8)
1. a polycrystalline silicon casting ingot process is characterized in that, this technological process may further comprise the steps:
S1, will scribble the crucible dehydration of silicon nitride coating after, the splendid attire polycrystalline silicon material also places ingot furnace;
S2, the temperature with ingot furnace in the Preset Time scope rise to sintering temperature, and keep the said sintering temperature scheduled time, so that said silicon nitride coating is sintered on the inwall of said crucible;
S3, the temperature in the ingot furnace is adjusted to said polycrystalline silicon material temperature of fusion, long brilliant temperature, annealing temperature, cooling temperature by sintering temperature successively, under relevant temperature, accomplishes the fusing of polysilicon, long crystalline substance, annealing, process for cooling respectively.
2. polycrystalline silicon casting ingot process as claimed in claim 1 is characterized in that, in said step S2, the scheduled time scope of keeping said sintering temperature is 45min～120min.
3. polycrystalline silicon casting ingot process as claimed in claim 2 is characterized in that, in said step S3, the time range that said sintering temperature is adjusted to said polycrystalline silicon material temperature of fusion is 300min～370min.
4. polycrystalline silicon casting ingot process as claimed in claim 3 is characterized in that, in said step S2, it is 0min～130min that said Preset Time is chosen scope.
5. like each described polycrystalline silicon casting ingot process of claim 1 to 4, it is characterized in that said sintering range is 800 ℃～1100 ℃.
6. polycrystalline silicon casting ingot process as claimed in claim 5 is characterized in that, in said step S1, the spraying coating process TR of said silicon nitride coating is 50 ℃～100 ℃.
7. polycrystalline silicon casting ingot process as claimed in claim 5 is characterized in that, before said step S1, also has following steps:
S0, outfit silicon nitride solution, the ratio range of silicon nitride and pure water is in the said silicon nitride solution: 0.2g/ml～0.27g/ml.
8. polycrystalline silicon casting ingot process as claimed in claim 1 is characterized in that, in said step S1, places air 0.5h～2h realization dehydration or places drying oven to realize dehydration through the crucible after will spraying.
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| CN2012102239427A CN102719889A (en) | 2012-06-27 | 2012-06-27 | Polysilicon ingot casting process |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102965727A (en) * | 2012-12-10 | 2013-03-13 | 英利能源（中国）有限公司 | Polycrystalline silicon ingot and casting method thereof |
| CN103628128A (en) * | 2013-12-12 | 2014-03-12 | 英利集团有限公司 | Crucible, production method of crucible and casting method of polycrystalline silicon ingot |
| CN107723793A (en) * | 2017-11-21 | 2018-02-23 | 浙江师范大学 | Crucible bottom heat conducting device and method for high quality polycrystalline silicon growth |
| CN109881249A (en) * | 2019-03-28 | 2019-06-14 | 晶科能源有限公司 | For the silica crucible of polycrystalline silicon ingot casting, ingot furnace and polycrystalline silicon ingot casting method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003041357A (en) * | 2001-07-27 | 2003-02-13 | Tocalo Co Ltd | Silicon holding vessel and manufacturing method therefor |
| CN101797544A (en) * | 2010-03-19 | 2010-08-11 | 常熟华融太阳能新型材料有限公司 | Automatic spraying device and automatic spraying process for solar energy quartz crucible |
| CN102021650A (en) * | 2010-12-31 | 2011-04-20 | 常州天合光能有限公司 | Production method of large polycrystalline ingot |
| CN102352531A (en) * | 2011-10-09 | 2012-02-15 | 泰州德通电气有限公司 | Crucible spraying free-sintering polycrystal ingot casting process |
-
2012
- 2012-06-27 CN CN2012102239427A patent/CN102719889A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003041357A (en) * | 2001-07-27 | 2003-02-13 | Tocalo Co Ltd | Silicon holding vessel and manufacturing method therefor |
| CN101797544A (en) * | 2010-03-19 | 2010-08-11 | 常熟华融太阳能新型材料有限公司 | Automatic spraying device and automatic spraying process for solar energy quartz crucible |
| CN102021650A (en) * | 2010-12-31 | 2011-04-20 | 常州天合光能有限公司 | Production method of large polycrystalline ingot |
| CN102352531A (en) * | 2011-10-09 | 2012-02-15 | 泰州德通电气有限公司 | Crucible spraying free-sintering polycrystal ingot casting process |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102965727A (en) * | 2012-12-10 | 2013-03-13 | 英利能源（中国）有限公司 | Polycrystalline silicon ingot and casting method thereof |
| CN102965727B (en) * | 2012-12-10 | 2015-05-13 | 英利能源（中国）有限公司 | Polycrystalline silicon ingot and casting method thereof |
| CN103628128A (en) * | 2013-12-12 | 2014-03-12 | 英利集团有限公司 | Crucible, production method of crucible and casting method of polycrystalline silicon ingot |
| CN103628128B (en) * | 2013-12-12 | 2016-06-15 | 英利集团有限公司 | Crucible and preparation method thereof, polycrystal silicon ingot casting method |
| CN107723793A (en) * | 2017-11-21 | 2018-02-23 | 浙江师范大学 | Crucible bottom heat conducting device and method for high quality polycrystalline silicon growth |
| CN109881249A (en) * | 2019-03-28 | 2019-06-14 | 晶科能源有限公司 | For the silica crucible of polycrystalline silicon ingot casting, ingot furnace and polycrystalline silicon ingot casting method |
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Application publication date: 20121010 |