CN102732948A - Method for improving ingot-casting monocrystaline silicon yield - Google Patents
Method for improving ingot-casting monocrystaline silicon yield Download PDFInfo
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- CN102732948A CN102732948A CN2012102052942A CN201210205294A CN102732948A CN 102732948 A CN102732948 A CN 102732948A CN 2012102052942 A CN2012102052942 A CN 2012102052942A CN 201210205294 A CN201210205294 A CN 201210205294A CN 102732948 A CN102732948 A CN 102732948A
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Abstract
The invention relates to a method for improving an ingot-casting monocrystaline silicon yield. The method is realized through the controlling over the diffusion of the impurities at the bottom of the crucible towards seed crystals. The method provided by the invention is based on the blocking upon the diffusion of the impurities at the bottom of the crucible towards the inner sides of the seed crystals. A barrier layer is arranged at the bottom of the seed crystals. The barrier layer comprises powdery, film, block or gap separations. Compared with ingot-casting monocrystaline with no diffusion barrier layer, the lifetime of the minority carrier on the bottom of the ingot-casting monocrystaline silicon ingot provided by the invention is substantially improved. According to a same truncation standard, the crystal ingot yield is improved by more than 3 percentage points (absolute difference).
Description
Technical field
The present invention relates to the photovoltaic cell field, especially a kind ofly the diffusion of contaminants blocking layer is set, stop the diffusion of impurity in crystal ingot, improve the method for ingot casting silicon single crystal yield with this in the ingot casting crucible bottom.
Background technology
Coming induced growth ingot casting silicon single crystal through the seed crystal with particular crystal orientation is to have obtained a kind of technology of significantly using in recent years in photovoltaic silion cell field, and the related patent U.S. Patent No. of having applied for has:
(1) mentions employing < 100>silicon single crystal among the patent US2007/0169685 (A1) and come induced growth ingot casting silicon single crystal, think that this kind technology can obviously reduce or eliminate defect concentration, obtain crystal grain at least greater than the crystal ingot of 10cm as seed crystal.
(2) inventor proposes the quartz plate of center drilling is placed crucible bottom among the patent CN201010284738.7, and quartz plate is the prismatoid structure, can save the seed crystal consumption.What grow out is < 100>crystal orientation monocrystalline.
(3) inventor proposes to adopt < 111>silicon single crystal to induce as seed crystal and generates the ingot casting silicon single crystal with < 111>crystal orientation among the patent CN 201010299013.5, because < 111>are the preferential growth directions, therefore can obtain a high proportion of ingot casting monocrystalline.
In the ingot casting single crystal growth process, induced growth can take place in the seed crystal partial melting on the solid-liquid interface of residue seed crystal and melted silicon liquid, and the class single crystal orientation that is grown is consistent with the seed crystal crystal orientation.The seed crystal of melt portions has not experienced the intensification of silicon material, fusing, long brilliant and annealing stage, and thermal history is longer than common ingot casting polycrystalline bottom silicon crystal far away.Experimental result shows that the yield of ingot casting silicon single crystal (per-cent) is lower than 5 ~ 8 percentage points of common ingot casting polysilicons, has increased the production cost of ingot casting silicon single crystal greatly.Crystal ingot bottom minority carrier life time is low to be to cause the low major cause of ingot casting monocrystalline yield.Such as, be the standard of blocking according to minority carrier life time 1 microsecond, the amount of blocking of ingot casting monocrystalline reaches 50 ~ 60mm, far above common ingot casting polycrystalline 15 ~ 25mm.Above-mentionedly be referred to as red sector in the truncation part industry, i.e. the undesirable part of minority carrier life time.
Through analyzing, the higher reason of ingot casting monocrystalline red sector is mainly from the diffusion of contaminants of crucible bottom.Ingot casting is much lower with the relative silicon material of the purity of quartz crucible, and the impurity in the crucible can diffuse into silicon crystal, reduces minority carrier life time widely as few sub-deathnium; The total amount of diffusion of contaminants entering silicon crystal and temperature and diffusion time are closely related; Temperature is high more, and the time is of a specified duration more, and the total impurities that diffuses into is big more; The low minority carrier life time zone that forms is many more, and the crystal ingot yield is low more.The thermal history of the residue seed crystal of ingot casting monocrystalline experience is longer, and the total impurities that is therefore diffused into is bigger, tends to be used as low minority carrier life time zone and is blocked.
Therefore, the control diffusion of crucible impurity in seed crystal is to improving ingot casting monocrystalline crystal ingot bottom minority carrier life time, reducing blocking length, improving the crystal ingot yield extremely important meaning is arranged of bottom red sector.
Summary of the invention
The technical problem that the present invention will solve is: propose a kind ofly can control the diffusion of crucible impurity in seed crystal, improve ingot casting monocrystalline crystal ingot bottom minority carrier life time, reduce the length of blocking of bottom red sector, improve the method for crystal ingot yield.
The technical scheme that the present invention adopted is: a kind of method that improves ingot casting silicon single crystal yield may further comprise the steps:
1) in the ingot casting crucible bottom diffusion of contaminants blocking layer is set, stops the diffusion of impurity in crystal ingot;
2) be that the monocrystalline silico briquette of 5 ~ 50 mm is closely arranged with thickness, be paved with crucible bottom as seed crystal;
3) successively silicon material, alloying element raw material are placed crucible then;
4) extracting vacuum and feed rare gas element N
2Or Ar, feed rare gas element while vacuumizing;
5) heating crucible, the part that makes monocrystalline silico briquette as seed crystal be contacted with crucible bottom does not melt, and all melts with the discontiguous part of crucible, silicon material and alloying element raw material and thorough mixing each other on atomic scale;
6) during directional freeze, making crucible bottom is cold junction, and the not melt portions of seed crystal is induced the growth of solidifying of silicon melt, obtains having the ingot casting silicon single crystal of particular crystal orientation.
Specifically, the diffusion of contaminants blocking layer in the step 1) according to the invention be silicon nitride film, silicon nitride powder, silicon nitride ball, quartz plate, porous silicon, silica flour, silicon chip, built on stilts or other have the form of diffusion of contaminants barrier functionality.Film or silicon chip are adopted in described diffusion of contaminants blocking layer, and thickness is 0.01 ~ 5mm; Adopt sheet material, thickness is 5 ~ 20mm; Adopt meal, pine dress thickness is 0.5 ~ 20mm; Adopt and make somebody a mere figurehead, then built on stilts height is 1 ~ 20mm.Described making somebody a mere figurehead achieved the goal through the supporter supports seed crystal.
Ingot casting monocrystalline of the present invention is meant and adopts single crystal seed inductive method, the monocrystalline that in the directional freeze process, is produced.Used crucible is including, but not limited to quartz crucible commonly used.Single crystal seed of the present invention is meant that the crystal orientation is that < 100 >, < 110 >, < 111 >, < 112>or mixed by above-mentioned crystal orientation seed crystal are spliced.
The invention has the beneficial effects as follows: based on to crucible bottom impurity to the stopping of seed crystal internal divergence, in the seed crystal bottom blocking layer is set; Compare the ingot casting monocrystalline that diffusion impervious layer is not set, the minority carrier life time of the ingot casting monocrystalline crystal ingot bottom that the present invention is prepared has obtained increasing substantially, and by the identical standard of blocking, the crystal ingot yield has improved (absolute difference) more than 3 percentage points.
Embodiment
Embodiment 1
With diameter be the silicon nitride ball close-packed of 6mm in crucible bottom, be covered with one deck, < 111>the seed crystal silico briquette that will be of a size of 330 * 150 mm is then closely arranged at quartz crucible bottom, thick 40 mm of seed crystal silico briquette.210kg silicon material places above the seed crystal silico briquette, mixes the doping agent boron of 40 mg, is adding 210kg silicon material, realizes shove charge.Burner hearth is evacuated, adopts Ar to do shielding gas.The design thermal field makes the silicon material portion temperature in the burner hearth reach more than 1420 ℃ and fusing gradually, makes interior < 111>silicon single crystal of burner hearth and silicon material contact part melt 20 mm, and 20 mm that contact with quartz crucible keep not melting.At last, open stay-warm case, silicon melt is solidified from crucible bottom gradually, rely on inducing of < 111>crystal orientation seed crystal and realize the oriented growth of silicon crystal obtaining the ingot casting monocrystalline.
Compare the ingot casting monocrystalline that crucible bottom is not placed with silicon nitride ball, low minority carrier life time district, bottom is all blocked according to 0.6 microsecond, and the bottom amount of blocking of present embodiment reduces to 30 mm by 45 original mm, and the crystal ingot yield brings up to 65% by 61%.
Embodiment 2
With thickness be 5mm, wide be that 10 mm, length are that the quartz bar of 400 mm is got 16; Evenly be laid on the crucible bottom that is of a size of 800 * 800 * 480 mm; Closely arrange < 100>the seed crystal silico briquette that is of a size of 400 * 400 mm on quartz plate thick 30 mm of seed crystal silico briquette then.210kg silicon material places above the seed crystal silico briquette, mixes the doping agent boron of 40 mg, is adding 210kg silicon material, realizes shove charge.Burner hearth is evacuated, adopts Ar to do shielding gas.The design thermal field makes the silicon material portion temperature in the burner hearth reach more than 1420 ℃ and fusing gradually, makes interior < 100>silicon single crystal of burner hearth and silicon material contact part melt 20 mm, and 10 mm that contact with quartz crucible keep not melting.At last, open stay-warm case, silicon melt is solidified from crucible bottom gradually, rely on inducing of < 100>crystal orientation seed crystal and realize the oriented growth of silicon crystal obtaining the ingot casting monocrystalline.
Compare the ingot casting monocrystalline that crucible bottom is not placed with quartz bar, low minority carrier life time district, bottom is all blocked according to 0.6 microsecond, and the bottom amount of blocking of present embodiment reduces to 20 mm by 40 original mm, and the crystal ingot yield brings up to 66% by 62%.
Embodiment 3
With particle diameter is that the high-purity silicon powder of 0.05mm is laid on crucible bottom, and the pine dress thickness of silica flour is 3 mm, closely arranges < 110>the seed crystal silico briquette that is of a size of 400 * 400 mm at quartz crucible bottom, thick 30 mm of seed crystal silico briquette then.210kg silicon material places above the seed crystal silico briquette, mixes the doping agent boron of 40 mg, is adding 210kg silicon material, realizes shove charge.Burner hearth is evacuated, adopts Ar to do shielding gas.The design thermal field makes the silicon material portion temperature in the burner hearth reach more than 1420 ℃ and fusing gradually, makes interior < 110>silicon single crystal of burner hearth and silicon material contact part melt 5 mm, and 20 mm that contact with silica flour keep not melting.At last, open stay-warm case, silicon melt is solidified from crucible bottom gradually, rely on inducing of < 110>crystal orientation seed crystal and realize the oriented growth of silicon crystal obtaining the ingot casting monocrystalline.
Compare the ingot casting monocrystalline that crucible bottom is not placed with high-purity silicon powder, low minority carrier life time district, bottom is all blocked according to 0.6 microsecond, and the bottom amount of blocking of present embodiment reduces to 25 mm by 45 original mm, and the crystal ingot yield brings up to 65.5% by 61%.
What describe in the above specification sheets is embodiment of the present invention; Various not illustrating constitutes restriction to flesh and blood of the present invention; Under the those of ordinary skill of technical field after having read specification sheets can to before described embodiment make an amendment or be out of shape, and do not deviate from essence of an invention and scope.
Claims (4)
1. method that improves ingot casting silicon single crystal yield is characterized in that may further comprise the steps:
1) in the ingot casting crucible bottom diffusion of contaminants blocking layer is set, stops the diffusion of impurity in crystal ingot;
2) be that the monocrystalline silico briquette of 5 ~ 50 mm is closely arranged with thickness, be paved with crucible bottom as seed crystal;
3) successively silicon material, alloying element raw material are placed crucible then;
4) extracting vacuum and feed rare gas element N
2Or Ar, feed rare gas element while vacuumizing;
5) heating crucible, the part that makes monocrystalline silico briquette as seed crystal be contacted with crucible bottom does not melt, and all melts with the discontiguous part of crucible, silicon material and alloying element raw material and thorough mixing each other on atomic scale;
6) during directional freeze, making crucible bottom is cold junction, and the not melt portions of seed crystal is induced the growth of solidifying of silicon melt, obtains having the ingot casting silicon single crystal of particular crystal orientation.
2. a kind of method that improves ingot casting silicon single crystal yield as claimed in claim 1 is characterized in that: the diffusion of contaminants blocking layer in the said step 1) be silicon nitride film, silicon nitride powder, silicon nitride ball, quartz plate, porous silicon, silica flour, silicon chip, built on stilts or other have the form of diffusion of contaminants barrier functionality.
3. a kind of method that improves ingot casting silicon single crystal yield as claimed in claim 2 is characterized in that: film or silicon chip are adopted in described diffusion of contaminants blocking layer, and thickness is 0.01 ~ 5mm; Adopt sheet material, thickness is 5 ~ 20mm; Adopt meal, pine dress thickness is 0.5 ~ 20mm; Adopt and make somebody a mere figurehead, then built on stilts height is 1 ~ 20mm.
4. a kind of method that improves ingot casting silicon single crystal yield as claimed in claim 3 is characterized in that: described making somebody a mere figurehead achieved the goal through the supporter supports seed crystal.
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Cited By (11)
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| WO2013149560A1 (en) * | 2012-04-01 | 2013-10-10 | 江西赛维Ldk太阳能高科技有限公司 | Polycrystalline silicon ingot, preparation method thereof, and polycrystalline silicon wafer |
| CN103882517A (en) * | 2014-04-04 | 2014-06-25 | 阿特斯(中国)投资有限公司 | Preparation method of polycrystalline silicon ingot |
| CN105603507A (en) * | 2016-02-03 | 2016-05-25 | 江西赛维Ldk太阳能高科技有限公司 | Seed crystal laying method, preparation method of monocrystalline silicon-like ingot and monocrystalline silicon-like piece |
| CN106521621A (en) * | 2016-09-20 | 2017-03-22 | 江西赛维Ldk太阳能高科技有限公司 | Ingot casting method capable of reducing red edge width of polycrystalline silicon ingot, polycrystalline silicon ingot and crucible for polycrystalline silicon ingot casting |
| CN106757331A (en) * | 2016-12-16 | 2017-05-31 | 江西赛维Ldk太阳能高科技有限公司 | A kind of polycrystal silicon ingot and preparation method thereof |
| CN108456930A (en) * | 2018-02-24 | 2018-08-28 | 常熟华融太阳能新型材料有限公司 | A kind of polycrystalline silicon ingot casting porous silicon seed and its preparation method and application |
| CN108588824A (en) * | 2018-06-12 | 2018-09-28 | 山东大海新能源发展有限公司 | The method for avoiding introducing impurity during crystal ingot casting using barrier |
| CN108754614A (en) * | 2018-06-28 | 2018-11-06 | 浙江大学 | A kind of quasi-monocrystalline silicon crucible for casting ingots using silica membrane as barrier layer |
| 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 |
| CN110534590A (en) * | 2019-08-16 | 2019-12-03 | 上海交通大学 | A kind of silicon nitride film and preparation method thereof improving solar cell long-wave response |
| CN111705358A (en) * | 2020-06-30 | 2020-09-25 | 江苏协鑫硅材料科技发展有限公司 | Cast monocrystalline silicon ingot and preparation method thereof |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2013149560A1 (en) * | 2012-04-01 | 2013-10-10 | 江西赛维Ldk太阳能高科技有限公司 | Polycrystalline silicon ingot, preparation method thereof, and polycrystalline silicon wafer |
| US10253430B2 (en) | 2012-04-01 | 2019-04-09 | Jiang Xi Sai Wei Ldk Solar Hi-Tech Co., Ltd. | Method for preparing polycrystalline silicon ingot |
| US10227711B2 (en) | 2012-04-01 | 2019-03-12 | Jiang Xi Sai Wei Ldk Solar Hi-Tech Co., Ltd. | Method for preparing polycrystalline silicon ingot |
| CN103882517A (en) * | 2014-04-04 | 2014-06-25 | 阿特斯(中国)投资有限公司 | Preparation method of polycrystalline silicon ingot |
| CN105603507A (en) * | 2016-02-03 | 2016-05-25 | 江西赛维Ldk太阳能高科技有限公司 | Seed crystal laying method, preparation method of monocrystalline silicon-like ingot and monocrystalline silicon-like piece |
| CN105603507B (en) * | 2016-02-03 | 2018-11-06 | 江西赛维Ldk太阳能高科技有限公司 | The preparation method and class monocrystalline silicon piece of a kind of laying method of seed crystal, class monocrystal silicon |
| CN106521621B (en) * | 2016-09-20 | 2019-01-29 | 江西赛维Ldk太阳能高科技有限公司 | A kind of casting ingot method, polycrystal silicon ingot and crucible used for polycrystalline silicon ingot casting reducing the red hem width degree of polycrystal silicon ingot |
| CN106521621A (en) * | 2016-09-20 | 2017-03-22 | 江西赛维Ldk太阳能高科技有限公司 | Ingot casting method capable of reducing red edge width of polycrystalline silicon ingot, polycrystalline silicon ingot and crucible for polycrystalline silicon ingot casting |
| CN106757331A (en) * | 2016-12-16 | 2017-05-31 | 江西赛维Ldk太阳能高科技有限公司 | A kind of polycrystal silicon ingot and preparation method thereof |
| CN106757331B (en) * | 2016-12-16 | 2019-03-08 | 赛维Ldk太阳能高科技(新余)有限公司 | A kind of polycrystal silicon ingot and preparation method thereof |
| CN108456930A (en) * | 2018-02-24 | 2018-08-28 | 常熟华融太阳能新型材料有限公司 | A kind of polycrystalline silicon ingot casting porous silicon seed and its preparation method and application |
| CN108588824A (en) * | 2018-06-12 | 2018-09-28 | 山东大海新能源发展有限公司 | The method for avoiding introducing impurity during crystal ingot casting using barrier |
| CN108754614A (en) * | 2018-06-28 | 2018-11-06 | 浙江大学 | A kind of quasi-monocrystalline silicon crucible for casting ingots using silica membrane as barrier layer |
| 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 |
| CN110534590A (en) * | 2019-08-16 | 2019-12-03 | 上海交通大学 | A kind of silicon nitride film and preparation method thereof improving solar cell long-wave response |
| CN111705358A (en) * | 2020-06-30 | 2020-09-25 | 江苏协鑫硅材料科技发展有限公司 | Cast monocrystalline silicon ingot and preparation method thereof |
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Application publication date: 20121017 |