CN104294355A - Polysilicon preparation process - Google Patents
Polysilicon preparation process Download PDFInfo
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- CN104294355A CN104294355A CN201410448605.7A CN201410448605A CN104294355A CN 104294355 A CN104294355 A CN 104294355A CN 201410448605 A CN201410448605 A CN 201410448605A CN 104294355 A CN104294355 A CN 104294355A
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- forming core
- core source
- layer forming
- crucible
- polycrystalline silicon
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Abstract
The invention discloses a polysilicon preparation process, which comprises the steps of: 1. laying a first layer of nucleation source evenly at the bottom of a crucible; 2. spraying a coating on the first layer of nucleation source to completely cover the first layer of nucleation source; 3. laying a second layer of nucleation source uniformly on the coating formed in step 2; 4. holding polysilicon in the crucible to finish charging; 5. placing the silicon material filled crucible in a polycrystalline ingot furnace to conduct vacuum pumping and heating, and then entering a high temperature melting stage, controlling the maximum melting temperature of the ingot furnace at 1510DEG C-1540DEG C, and adjusting the thermal field to keep top-down melting of the polycrystalline silicon material; 6. measuring the height of the nucleation source through a high purity quartz rod, and entering a crystal growth stage when the residual amount of the second layer of nucleation source is 0cm; and 7. subjecting the silicon material to crystal growth, annealing and cooling, thus obtaining a polysilicon ingot. According to the process provided by the invention, the polysilicon ingot with uniform and fine crystalline grains can be obtained, and the polysilicon ingot has the characteristics of long bottom minority carrier lifetime, low impurity rate and high yield, etc.
Description
Technical field
The invention belongs to field of photovoltaic technology, be specifically related to a kind of polycrystalline silicon preparing process.
Background technology
The continuous exhaustion of Nonrenewable energy resources makes renewable energy source receive to pay close attention to widely, and solar electrical energy generation expands ratio shared in global generated energy gradually, and crystalline silicon becomes current most important solar energy photovoltaic material.
But at present, traditional polycrystal silicon ingot forging type is subject to many-sided restriction, its make after the working efficiency of polysilicon chip general lower, during conventional multi-crystalline silicon ingot casting, by directional solidification technique, adopt crucible dress silicon material, by the heating to silicon material, fusing, long crystalline substance, annealing and cooling step, obtain polycrystal silicon ingot, silicon material, in melting situation, enters the long brilliant stage, by the cooling of crucible bottom, production nucleus spontaneous at random, and grow on this basis.This kind of nucleus is spontaneous at random due to it, easily produces various defect, causes the polysilicon chip quality made not high.
In order to the growth of nucleus effectively can be controlled, researchist is had to pass through to adopt crucible bottom to lay the forming core source as silicon ingot growth such as monocrystalline silico briquette, single polycrystalline chip, particle small powder, by controlled melting speed, the basis that forming core source is not completely melted grows, obtain the polycrystal silicon ingot of low defect high-quality, but the method has following shortcoming:
1. crucible bottom forming core source is not completely melted, and the low minority carrier life time region bottom the polycrystal silicon ingot made increases, and reduces the yield rate of silicon ingot;
2. bottom, forming core source is not melted, and cannot volatilize completely in the partial impurities source of existence, the percentage of admixture of the polycrystal silicon ingot inside of making is raised, affects the quality of polycrystal silicon ingot.
Forming core source, by adopting in crucible manufacturing processed, is fixed on crucible bottom by existing researchist, obtained the polycrystal silicon ingot of high-quality, but the method has following shortcoming by the forming core source of crucible bottom:
1. bottom, forming core source easily causes polycrystal silicon ingot to glue pot crackle;
2. bottom, forming core source distribution is uneven, and polycrystal silicon ingot quality declines.
For solving the defect that single fine melt forming core source or single fritting forming core source cause, therefore needing a kind of new technical scheme, improving polycrystal silicon ingot quality and improving yield rate.
Summary of the invention
Goal of the invention: for above-mentioned prior art Problems existing and deficiency, the object of this invention is to provide a kind of polycrystalline silicon preparing process, this technique comprises the advantage that polycrystal silicon ingot is prepared in fine melt and fritting forming core source, under the prerequisite promoting polycrystal silicon ingot quality, by technique adjustment, effectively promote the yield rate of polycrystal silicon ingot.
Technical scheme: the invention discloses a kind of polycrystalline silicon preparing process, comprise the following steps:
1. evenly lay the first layer forming core source in crucible bottom;
2. on the first layer forming core source, be coated with sprayed coating, coating complete covering the first layer forming core source;
3. in the coating of step 2, evenly lay second layer forming core source;
4. by polycrystalline silicon material splendid attire in crucible, complete charging;
5. the crucible filling silicon material is placed in polycrystalline ingot furnace, carry out vacuumizing, heating, and then entering the high temperature melting stage, the maximum temperature of fusion of described ingot furnace controls at 1510 DEG C-1540 DEG C, and keeps polycrystalline silicon material to melt from top to bottom by adjustment thermal field;
6. by high purity quartz rod, forming core source height is measured, when the residual content in second layer forming core source is 0cm, and then enter the long brilliant stage;
7. silicon material is through long crystalline substance, annealing, cooling, obtains polycrystal silicon ingot.
Wherein, the first layer forming core source quality of the present invention is not less than 500g, and second layer forming core source quality is not less than 30kg.
The present invention is by before the silicon material fusing later stage enters the long crystalline substance initial stage, by high purity quartz rod, the height in forming core source is measured, when making the residual content in forming core source just reach 0cm, reduce ingot casting in-furnace temperature, second layer forming core source is made no longer to continue fusing, now second layer forming core source is in just fusing end and no longer continues fusing, enter long brilliant with this state, second layer forming core source under this state contacts with the first layer forming core source, the acting in conjunction when long brilliant initial stage forming core, obtains high-quality polycrystal silicon ingot; But when second layer forming core source is not in optimal morphology, long brilliant initial stage forming core will be acted on by the first layer forming core source, still can obtain higher quality polycrystal silicon ingot.
As further optimization of the present invention, the first layer forming core source of the present invention and second layer forming core source are silicon material, and its structure is single crystal structure, its shape can be bulk, sheet, particulate state or Powdered, forming core source of the present invention is laid should be even, and gap, forming core source is identical, and densification is redundancy not.
As further optimization of the present invention, adopt quartz pushrod to measure forming core source residual content in step 6 of the present invention, the present invention also controls forming core source burn-off rate by quartz pushrod testing method.
As further optimization of the present invention, the first layer forming core source of the present invention order number is greater than an order.
As further optimization of the present invention, crucible of the present invention is square quartz crucible.
As further optimization of the present invention, second layer forming core source of the present invention silicon material is single crystal structure.
As further optimization of the present invention, coating of the present invention is silicon nitride coating.
Beneficial effect: the present invention compared with prior art, has the following advantages:
1, a kind of polycrystalline silicon preparing process provided by the invention, can obtain the polycrystal silicon ingot of uniform crystal particles exquisiteness, have defect less, bottom polycrystal silicon ingot, minority carrier life time is long, and percentage of admixture is low, yield rate high.
2, the present invention is under the prerequisite obtaining high-quality silicon ingot, and manufacturing cost reduces, and has good economic benefit.
Embodiment
The present invention is illustrated further below in conjunction with embodiment.
Embodiment 1:
The present embodiment selection standard G6 square quartz crucible is that the silicon material of 500g diameter 4mm is as the first layer forming core source at quartz crucible bottom even laying quality; Even application silicon nitride on the first layer forming core source, makes the complete coated the first layer forming core source of silicon nitride coating; Silicon nitride coating is evenly laid broken virgin polycrystalline silicon material as second layer forming core source, quality 30kg; Polycrystalline silicon material splendid attire is completed charging in square crucible; The square crucible filling silicon material is placed in polycrystalline cast ingot table, carry out vacuumizing, heating, make it to enter the high temperature melting stage, the maximum temperature of fusion of polycrystalline silicon ingot or purifying furnace controls at 1540 DEG C, keeps polycrystalline silicon material to melt from top to bottom by adjustment thermal field, adopts the mode of quartz pushrod test to control the burn-off rate of silicon material, as the solid-liquid interface distance square quartz crucible bottom distance residue 15mm of silicon material, reduce the temperature of polycrystal silicon ingot stove, be reduced to 1430 DEG C, and then enter the long brilliant stage.
Through long crystalline substance, annealing and cooling stages, obtain high-quality polycrystal silicon ingot, gained silicon ingot obtains 36 pieces of silico briquettes through evolution, obtains polysilicon chip through section cleaning.
Comparative example 1:
Employing standard G6 square quartz crucible, the broken virgin polycrystalline silicon material of 30kg is evenly laid in crucible bottom, again polycrystalline silicon material splendid attire is completed charging in square crucible, the crucible filling silicon material is placed in polycrystalline silicon ingot casting table, carry out vacuumizing, heating, make it to enter the high temperature melting stage, the maximum temperature of fusion of polycrystalline silicon ingot or purifying furnace controls at 1540 DEG C, thermal field is regulated to keep polycrystalline silicon material to melt from top to bottom, adopt quartz pushrod metering system to control silicon material burn-off rate, when silicon material no longer melts, reduce temperature to 1430 DEG C, enter the long brilliant stage.
Through long crystalline substance, annealing and cooling stages, obtain polycrystal silicon ingot, gained silicon ingot is carried out evolution and obtain 36 pieces of silico briquettes, obtain polysilicon chip through section, cleaning.
Comparative example 2:
Selection standard G6 square quartz crucible, the silicon material 500g of diameter 4mm is laid at quartz crucible bottom even, spraying silicon nitride on silicon material, make silicon nitride coating complete covering bottom silicon material, again by polycrystalline silicon material splendid attire in square crucible, complete charging work, the crucible filling silicon material is placed in polycrystalline silicon ingot casting table, vacuumize, heating, make it to enter the high temperature melting stage, the maximum temperature of fusion of polycrystalline silicon ingot or purifying furnace controls at 1540 DEG C, thermal field is regulated to keep polycrystalline silicon material to be melted to from top to bottom after silicon material melts completely, reduce ingot furnace temperature to 1430 DEG C, and then enter the long brilliant stage.
Through long crystalline substance, annealing and cooling stages, obtain polycrystal silicon ingot, gained silicon ingot is carried out evolution and obtain 36 pieces of silico briquettes, obtain polysilicon chip through section, cleaning.
The yield rate of embodiment 1 and comparative example 1 and comparative example 2 gained polycrystal silicon ingot and polysilicon chip make the efficiency comparative's result after battery as table 1:
The yield rate that table 1 is embodiment 1 and comparative example 1,2 gained polycrystal silicon ingot and polysilicon chip make the efficiency comparative after cell piece
| Silicon ingot yield rate | Battery efficiency | |
| Embodiment 1 | 69.5％ | 18.05％ |
| Comparative example 1 | 67.5％ | 18.12％ |
| Comparative example 2 | 70.8％ | 17.94％ |
Comparative analysis can obtain: the silicon ingot yield rate of embodiment 1 comparatively comparative example 1 improves 2.0%; The battery efficiency of embodiment 1 comparatively comparative example 1 reduces by 0.%.The silicon ingot yield rate of embodiment 1 comparatively comparative example 2 reduces by 0.7%, and the battery efficiency of embodiment comparatively comparative example 2 improves 0.06%.
Embodiment 2
The present embodiment adopts standard G6 square quartz crucible, 200g silica flour is laid as the first layer forming core source at quartz crucible bottom even, even application silicon nitride on the first layer forming core source, make silicon nitride coating complete covering the first layer forming core source, silicon nitride coating evenly lays 50kg polycrystalline particle, again by polycrystalline silicon material splendid attire in square crucible, complete charging, the crucible filling silicon material is placed in polycrystalline silicon ingot casting table, vacuumize, heating, make it to enter the high temperature melting stage, the maximum temperature of fusion of polycrystalline silicon ingot or purifying furnace controls at 1510 DEG C, thermal field is regulated to keep polycrystalline silicon material to melt from top to bottom, quartz pushrod metering system is adopted to control the burn-off rate of silicon material, when the distance of the solid-liquid interface distance square quartz crucible bottom of silicon material is 5mm, reduce ingot furnace temperature, when silicon material solid-liquid interface just reaches contact crucible bottom, regulate the temperature of polycrystalline silicon ingot or purifying furnace, when the temperature of ingot furnace is reduced to, and then enter the long brilliant stage.
Through long crystalline substance, annealing and cooling stages, obtain polycrystal silicon ingot, gained silicon ingot is carried out evolution and obtain 36 pieces of silico briquettes, obtain polysilicon chip through section, cleaning.
The yield rate of the present embodiment gained polycrystal silicon ingot is 70.5%, and its battery efficiency making battery is 18.12%.
Claims (7)
1. a polycrystalline silicon preparing process, is characterized in that: comprise the following steps:
1. evenly lay the first layer forming core source in crucible bottom;
2. on the first layer forming core source, be coated with sprayed coating, coating complete covering the first layer forming core source;
3. in the coating of step 2, evenly lay second layer forming core source;
4. by polycrystalline silicon material splendid attire in crucible, complete charging;
5. the crucible filling silicon material is placed in polycrystalline ingot furnace, carries out vacuumizing, heating, and then enter the high temperature melting stage, the maximum temperature of fusion of described ingot furnace controls at 1510 DEG C-1540 DEG C, keeps polycrystalline silicon material to melt from top to bottom by adjustment thermal field;
6. when the residual content in second layer forming core source is 0cm, and then enter the long brilliant stage;
7. silicon material is through long crystalline substance, annealing, cooling, obtains polycrystal silicon ingot.
2. a kind of polycrystalline silicon preparing process according to claim 1, is characterized in that: described the first layer forming core source and second layer forming core source are silicon material.
3. a kind of polycrystalline silicon preparing process according to claim 1, is characterized in that: adopt quartz pushrod to measure forming core source residual content in described step 6.
4. a kind of polycrystalline silicon preparing process according to claim 1 and 2, is characterized in that: described the first layer forming core source order number is greater than an order.
5. a kind of polycrystalline silicon preparing process according to claim 1, is characterized in that: described crucible is square quartz crucible.
6. a kind of polycrystalline silicon preparing process according to claim 2, is characterized in that: described second layer forming core source silicon material is single crystal structure.
7. a kind of polycrystalline silicon preparing process according to claim 1, is characterized in that: described coating is silicon nitride coating.
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| CN201410448605.7A CN104294355A (en) | 2014-09-04 | 2014-09-04 | Polysilicon preparation process |
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| CN201410448605.7A CN104294355A (en) | 2014-09-04 | 2014-09-04 | Polysilicon preparation process |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104831349A (en) * | 2015-05-26 | 2015-08-12 | 江西旭阳雷迪高科技股份有限公司 | Method for increasing silicon slice quality through polycrystalline silicon ingot casting |
| CN105177710A (en) * | 2015-10-28 | 2015-12-23 | 镇江环太硅科技有限公司 | Manufacturing method for novel full-melting efficient crucible |
| CN105332049A (en) * | 2015-10-29 | 2016-02-17 | 镇江环太硅科技有限公司 | Preparation method of G6 low-impurity-diffusion low-dislocation-density high-purity efficient crucible |
| CN106012005A (en) * | 2016-07-13 | 2016-10-12 | 江苏协鑫硅材料科技发展有限公司 | Measuring quartz rod |
| CN109778311A (en) * | 2019-01-24 | 2019-05-21 | 赛维Ldk太阳能高科技(新余)有限公司 | A kind of preparation method and crucible for casting ingots of silicon ingot |
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| JP2011201737A (en) * | 2010-03-26 | 2011-10-13 | Mitsubishi Materials Corp | Manufacturing method for polycrystalline silicon ingot, and the polycrystalline silicon ingot |
| CN203485502U (en) * | 2013-07-30 | 2014-03-19 | 东海晶澳太阳能科技有限公司 | Quartz crucible coating for producing high-performance polycrystalline silicon ingot |
| CN103966664A (en) * | 2014-04-10 | 2014-08-06 | 晶海洋半导体材料（东海）有限公司 | Heterogenous coating crucible for polycrystal ingotting and preparation method of heterogenous coating crucible |
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2014
- 2014-09-04 CN CN201410448605.7A patent/CN104294355A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011201737A (en) * | 2010-03-26 | 2011-10-13 | Mitsubishi Materials Corp | Manufacturing method for polycrystalline silicon ingot, and the polycrystalline silicon ingot |
| CN203485502U (en) * | 2013-07-30 | 2014-03-19 | 东海晶澳太阳能科技有限公司 | Quartz crucible coating for producing high-performance polycrystalline silicon ingot |
| CN103966664A (en) * | 2014-04-10 | 2014-08-06 | 晶海洋半导体材料（东海）有限公司 | Heterogenous coating crucible for polycrystal ingotting and preparation method of heterogenous coating crucible |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104831349A (en) * | 2015-05-26 | 2015-08-12 | 江西旭阳雷迪高科技股份有限公司 | Method for increasing silicon slice quality through polycrystalline silicon ingot casting |
| CN105177710A (en) * | 2015-10-28 | 2015-12-23 | 镇江环太硅科技有限公司 | Manufacturing method for novel full-melting efficient crucible |
| CN105332049A (en) * | 2015-10-29 | 2016-02-17 | 镇江环太硅科技有限公司 | Preparation method of G6 low-impurity-diffusion low-dislocation-density high-purity efficient crucible |
| CN106012005A (en) * | 2016-07-13 | 2016-10-12 | 江苏协鑫硅材料科技发展有限公司 | Measuring quartz rod |
| CN109778311A (en) * | 2019-01-24 | 2019-05-21 | 赛维Ldk太阳能高科技(新余)有限公司 | A kind of preparation method and crucible for casting ingots of silicon ingot |
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Application publication date: 20150121 |