CN103318895B - A kind of method removing foreign matter of phosphor in silicon - Google Patents
A kind of method removing foreign matter of phosphor in silicon Download PDFInfo
- Publication number
- CN103318895B CN103318895B CN201310281112.4A CN201310281112A CN103318895B CN 103318895 B CN103318895 B CN 103318895B CN 201310281112 A CN201310281112 A CN 201310281112A CN 103318895 B CN103318895 B CN 103318895B
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- silicon
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- foreign matter
- phosphor
- silicon melt
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- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 124
- 239000010703 silicon Substances 0.000 title claims abstract description 124
- OAICVXFJPJFONN-UHFFFAOYSA-N phosphorus Chemical compound 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[P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 45
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N silicon Chemical compound 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- 239000002253 acid Substances 0.000 claims description 8
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[Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 2
- 229910052791 calcium Inorganic materials 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 238000005516 engineering process Methods 0.000 abstract description 5
- 238000002386 leaching Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 229910004706 CaSi2 Inorganic materials 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000000875 corresponding Effects 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
Abstract
The present invention relates to a kind of method removing foreign matter of phosphor in silicon, belong to silicon product deep process technology field.First in the industrial silicon melt carrying out external refining, add silicocalcium, obtain special composition silicon melt, after treating external refining, special composition silicon melt is cast; Special composition silicon melt after having cast is solidified by controlled, segmentation and condenses to room temperature, finally obtain special composition silicon product; Special composition silicon product can be obtained special composition silicon product powder after finishing, fragmentation, ball milling, screening, magnetic separation process process; Special composition silicon product powder is joined acidleach in acidic solution, finally can obtain low-phosphorous silicon product.The method has operational safety, easily controls, and the removal efficiency of foreign matter of phosphor is high, and can be combined with existing industrial silicon production process, production cost is low, is easy to advantages such as accomplishing scale production.
Description
Technical field
The present invention relates to a kind of method removing foreign matter of phosphor in silicon, belong to silicon product deep process technology field.
Background technology
Phosphorus is the element of a kind of important impurity in silicon, has obvious impact to the efficiency of conversion of solar cell.Prepare in solar-grade polysilicon novel process in metallurgy method, in order to remove foreign matter of phosphor, people take multiple method or means.Because the vapour pressure of phosphorus is higher, adopt vacuum volatilization dephosphorization to become one of focus of people's research, also achieve good progress.The Marvin's of Kunming University of Science and Technology can wait people to adopt vacuum distillation technique, carry out volatilization to the phosphorus in industrial silicon to remove, phosphorus content can be reduced to below 1ppmw, Dalian University of Technology and external numerous research institution all adopt electron beam to be studied the removal of foreign matter of phosphor in silicon, also good effect is all achieved, phosphorus can be reduced to below 0.5ppmw, the people such as the Zheng Songsheng of Xiamen University have carried out systematic study to vacuum dephosphorization process and dephosphorization mechanism, under 1823K, 0.08 ~ 0.15Pa vacuum tightness, can by phosphorus from 15 × 10
-4% is reduced to 12 × 10
-5%.Although the foreign matter of phosphor that vacuum volatilization is removed in silicon is a kind of effective method, but owing to needing to keep the condition of high temperature for a long time in the volatilization process of foreign matter of phosphor, energy expenditure is larger, base metal silicon also has corresponding loss, and the treatment capacity that what is more important vacuum method removes the foreign matter of phosphor in silicon is less, industrialized extensive process can not be adapted to, therefore cannot industrial applications.
The result of study of the people such as Morita shows, the foreign matter of phosphor in silicon can be enriched in by CaSi
2in the secondary sedimentation mutually formed, wet-leaching can be adopted to remove foreign matter of phosphor in silicon.The research of the people such as T.Shimpo shows, employing wet processing can by the Impurity removal 80% in silicon.Although adopt the method for wet-leaching the foreign matter of phosphor in silicon can be obtained the removal of part, but exist and be in the experimental study stage, there is the problems such as certain danger in the interpolation of Ca, has had a strong impact on progress and industrial applications that wet-leaching removes foreign matter of phosphor in silicon.
Summary of the invention
The present invention is exactly for above-mentioned prior art Problems existing and deficiency; a kind of method removing foreign matter of phosphor in silicon is provided; the method has operational safety; easy control; the removal efficiency of foreign matter of phosphor is high; can be combined with existing industrial silicon production process, production cost is low, is easy to advantages such as accomplishing scale production.
Remove a method for foreign matter of phosphor in silicon, concrete steps are as follows:
(1) to carrying out external refining, temperature adds silicocalcium higher than in the industrial silicon melt of 1600 DEG C, obtain special composition silicon melt, after treating 2 ~ 4h external refining, special composition silicon melt cast;
(2) the special composition silicon melt that step (1) obtains is carried out controlled, segmentation to solidify: first by special composition silicon melt with the condensing rate condensation of 0.1 ~ 5 DEG C/min, then when temperature drops to 1000 ~ 1400 DEG C, condensing rate is with 5 ~ 20 DEG C/min condensation, finally when temperature drops to below 1000 DEG C, special composition silicon melt is naturally cooled to room temperature, final acquisition special composition silicon product;
(3) the special composition silicon product in step (2) is obtained after finishing, fragmentation, ball milling, screening, magnetic separation process iron level and be less than 0.1wt% and granularity is 50 ~ 500 object special composition silicon product powders;
(4) be that (2 ~ 8): 1mL/g joins acidleach 6 ~ 24h in the acidic solution of 20 ~ 85 DEG C by step (3) gained special composition silicon product powder by liquid-solid ratio, finally obtain low-phosphorous silicon product (P content is less than 5ppmw).
In described step (1), the content of the impurity F e of industrial silicon melt is less than 0.2wt%, and P content is greater than 50ppmw.
Foreign matter content in described step (1) in silicocalcium meets the requirement in silicocalcium product national standard YB/T5061-2007.
In described step (1), the add-on of silicocalcium is added according to the requirement of calcium contents in special composition silicon melt, and add-on is no more than 20% of industrial silicon melt quality.
Being incorporated as of silicocalcium disposablely adds or multiple batches ofly to add in described step (1).
Described step (3) finishing, fragmentation, ball milling, screening, magnetic separation process require to carry out one or many process to special composition silicon product according to the granularity of special composition silicon product powder and iron level, or intersect or re-treatment.
Acidic solution in described step (4) is HCl, HNO
3, H
2sO
4in one or more arbitrary proportion mixing acid, wherein acid concentration be 1 ~ 8mol/L.
Acidleach in described step (4) is that multistage leaches, until the clearance of phosphorus is higher than 90%.
In removal silicon of the present invention, the method beneficial effect of foreign matter of phosphor is:
(1) the method can remove the foreign matter of phosphor in silicon in enormous quantities, is easier to accomplish scale production, industrially has a extensive future;
(2) this method eliminates the Hazard Factor that in existing wet method dephosphorization process, Ca adds, operate safer and more easily control;
(3) the method production cost is lower, effectively improves state of the art and the quality product of existing industrial silicon industry, promotes silicon value-added content of product, improves benefit and the social benefit of the economy of enterprise.
(4) in the low-phosphorous silicon product adopting the method finally to obtain, P content is less than 5ppmw, and the clearance of phosphorus is higher than 90%.
Accompanying drawing explanation
Fig. 1 is the process flow sheet that the present invention removes the method for foreign matter of phosphor in silicon.
Embodiment
Below in conjunction with accompanying drawing 1 and embodiment, the invention will be further described.
Embodiment 1
As Fig. 1 removes shown in the process flow sheet of the method for foreign matter of phosphor in silicon:
(1) to carrying out external refining, higher than the 1000kg industrial silicon melt of 1600 DEG C, (content of impurity F e is less than 0.2wt% to temperature, P content is higher than 50ppmw) in the disposable 100kg of adding meet the silicocalcium of national standard YB/T5061-2007, obtain special composition silicon melt, after treating 2h external refining, special composition silicon melt is cast;
(2) the special composition silicon melt obtained in step (1) is carried out controlled, segmentation to solidify: first by special composition silicon melt with the condensing rate condensation of 0.1 DEG C/min, then when temperature drops to 1000 DEG C, condensing rate is with 5 DEG C/min condensation, finally when temperature drops to 1000 DEG C, special composition silicon melt is naturally cooled to room temperature, final acquisition special composition silicon product;
(3) the special composition silicon product in step (2) is obtained iron level 0.09wt% after finishing, fragmentation, ball milling, screening, magnetic separation primary treatment and granularity is 50 object special composition silicon product powders;
(4) be that 2:1mL/g joins 20 DEG C, acidleach 6h in the HCl acidic solution of 1mol/L by step (3) gained special composition silicon product powder by liquid-solid ratio, acidleach is four sections of leachings, until the clearance of phosphorus is higher than 90% acidleach, the low-phosphorous silicon product of final acquisition (P content is 3ppmw).
Embodiment 2
As Fig. 1 removes shown in the process flow sheet of the method for foreign matter of phosphor in silicon:
(1) to carrying out external refining, higher than the 1000kg industrial silicon melt of 1600 DEG C, (content of impurity F e is less than 0.2wt% to temperature, P content is higher than 50ppmw) in add the silicocalcium that 150kg meets national standard YB/T5061-2007 at twice, obtain special composition silicon melt, after treating 4h external refining, special composition silicon melt is cast;
(2) the special composition silicon melt obtained in step (1) is carried out controlled, segmentation to solidify: first by special composition silicon melt with the condensing rate condensation of 3 DEG C/min, then when temperature drops to 1400 DEG C, condensing rate is with 15 DEG C/min condensation, finally when temperature drops to 900 DEG C, special composition silicon melt is naturally cooled to room temperature, final acquisition special composition silicon product;
(3) the special composition silicon product in step (2) is obtained iron level 0.07wt% after finishing, fragmentation, ball milling, screening, magnetic separation three times process and granularity is 500 object special composition silicon product powders;
(4) be that 8:1mL/g joins 85 DEG C, acidleach 12h in the mixed acid solution of 8mol/L by step (3) gained special composition silicon product powder by liquid-solid ratio, wherein HCl and the HNO of mixed acid solution to be volume ratio be 1:1
3mixed acid solution, acidleach is three stages acid leach, until the clearance of phosphorus is higher than 90% acidleach, the low-phosphorous silicon product of final acquisition (P content is 1ppmw).
Embodiment 3
As Fig. 1 removes shown in the process flow sheet of the method for foreign matter of phosphor in silicon:
(1) to carrying out external refining, higher than the 1000kg industrial silicon melt of 1600 DEG C, (content of impurity F e is less than 0.2wt% to temperature, P content is higher than 50ppmw) in the disposable 180kg of adding meet the silicocalcium of national standard YB/T5061-2007, obtain special composition silicon melt, after treating 3h external refining, special composition silicon melt is cast;
(2) the special composition silicon melt obtained in step (1) is carried out controlled, segmentation to solidify: first by special composition silicon melt with the condensing rate condensation of 5 DEG C/min, then when temperature drops to 1200 DEG C, condensing rate is with 20 DEG C/min condensation, finally when temperature drops to 800 DEG C, special composition silicon melt is naturally cooled to room temperature, final acquisition special composition silicon product;
(3) the special composition silicon product in step (2) is obtained iron level 0.08wt% after finishing, fragmentation, ball milling, screening, magnetic separation process twice and granularity is 300 object special composition silicon product powders;
(4) be that 6:1mL/g joins 80 DEG C, 6mol/LH by step (3) gained special composition silicon product powder by liquid-solid ratio
2sO
4acidleach 24h in acidic solution, acidleach is two sections of leachings, until the clearance of phosphorus is higher than 90% acidleach, the low-phosphorous silicon product of final acquisition (P content is 5ppmw).
Embodiment 4
As Fig. 1 removes shown in the process flow sheet of the method for foreign matter of phosphor in silicon:
(1) to carrying out external refining, higher than the 1000kg industrial silicon melt of 1600 DEG C, (content of impurity F e is less than 0.2wt% to temperature, P content is higher than 50ppmw) in the disposable 180kg of adding meet the silicocalcium of national standard YB/T5061-2007, obtain special composition silicon melt, after treating 3h external refining, special composition silicon melt is cast;
(2) the special composition silicon melt obtained in step (1) is carried out controlled, segmentation to solidify: first by special composition silicon melt with the condensing rate condensation of 5 DEG C/min, then when temperature drops to 1200 DEG C, condensing rate is with 20 DEG C/min condensation, finally when temperature drops to 800 DEG C, special composition silicon melt is naturally cooled to room temperature, final acquisition special composition silicon product;
(3) the special composition silicon product in step (2) is obtained after finishing, fragmentation, ball milling, screening, magnetic separation process twice iron level and be less than 0.1wt% and granularity is 300 object special composition silicon product powders;
(4) be that 6:1mL/g joins 80 DEG C, 6mol/LH by step (3) gained special composition silicon product powder by liquid-solid ratio
2sO
4acidleach 24h in acidic solution, acidleach is two sections of leachings, until the clearance of phosphorus is higher than 90% acidleach, the low-phosphorous silicon product of final acquisition (P content is 5ppmw).
Claims (8)
1. remove a method for foreign matter of phosphor in silicon, it is characterized in that concrete steps are as follows:
(1) to carrying out external refining, temperature adds silicocalcium higher than in the industrial silicon melt of 1600 DEG C, obtain special composition silicon melt, after treating 2 ~ 4h external refining, special composition silicon melt cast;
(2) the special composition silicon melt that step (1) obtains is carried out controlled, segmentation to solidify: first by special composition silicon melt with the condensing rate condensation of 0.1 ~ 5 DEG C/min, then when temperature drops to 1000 ~ 1400 DEG C, condensing rate is with 5 ~ 20 DEG C/min condensation, finally when temperature drops to below 1000 DEG C, special composition silicon melt is naturally cooled to room temperature, final acquisition special composition silicon product;
(3) the special composition silicon product in step (2) is obtained after finishing, fragmentation, ball milling, screening, magnetic separation process iron level and be less than 0.1wt% and granularity is 50 ~ 500 object special composition silicon product powders;
(4) be that 2 ~ 8:1mL/g joins acidleach 6 ~ 24h in the acidic solution of 20 ~ 85 DEG C by step (3) gained special composition silicon product powder by liquid-solid ratio, finally obtain low-phosphorous silicon product.
2. remove the method for foreign matter of phosphor in silicon according to claim 1, it is characterized in that: in described step (1), the content of the impurity F e of industrial silicon melt is less than 0.2wt%, and P content is greater than 50ppmw.
3. remove the method for foreign matter of phosphor in silicon according to claim 1, it is characterized in that: the foreign matter content in described step (1) in silicocalcium meets the requirement in silicocalcium product national standard YB/T5061-2007.
4. remove the method for foreign matter of phosphor in silicon according to claim 1, it is characterized in that: in described step (1), the add-on of silicocalcium is added according to the requirement of calcium contents in special composition silicon melt, and add-on is no more than 20% of industrial silicon melt quality.
5. remove the method for foreign matter of phosphor in silicon according to claim 1, it is characterized in that: in described step (1), being incorporated as of silicocalcium disposablely adds or multiple batches ofly to add.
6. remove the method for foreign matter of phosphor in silicon according to claim 1, it is characterized in that: described step (3) finishing, fragmentation, ball milling, screening, magnetic separation process require to carry out one or many process to special composition silicon product according to the granularity of special composition silicon product powder and iron level, or intersect or re-treatment.
7. remove the method for foreign matter of phosphor in silicon according to claim 1, it is characterized in that: the acidic solution in described step (4) is HCl, HNO
3, H
2sO
4in one or more arbitrary proportion mixing acid, wherein acid concentration be 1 ~ 8mol/L.
8. remove the method for foreign matter of phosphor in silicon according to claim 1, it is characterized in that: the acidleach in described step (4) is that multistage leaches, until the clearance of phosphorus is higher than 90%.
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| US4539194A (en) * | 1983-02-07 | 1985-09-03 | Elkem A/S | Method for production of pure silicon |
| CN101555013A (en) * | 2009-05-18 | 2009-10-14 | 贵阳宝源阳光硅业有限公司 | Refining method of industrial silicon |
| CN102020278A (en) * | 2009-09-09 | 2011-04-20 | 贵阳宝源阳光硅业有限公司 | Method for removing impurity phosphorus in silicon |
| CN102616787A (en) * | 2012-03-22 | 2012-08-01 | 厦门大学 | Method for removing boron-phosphorus impurities from silicon metal |
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Patent Citations (4)
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|---|---|---|---|---|
| US4539194A (en) * | 1983-02-07 | 1985-09-03 | Elkem A/S | Method for production of pure silicon |
| CN101555013A (en) * | 2009-05-18 | 2009-10-14 | 贵阳宝源阳光硅业有限公司 | Refining method of industrial silicon |
| CN102020278A (en) * | 2009-09-09 | 2011-04-20 | 贵阳宝源阳光硅业有限公司 | Method for removing impurity phosphorus in silicon |
| CN102616787A (en) * | 2012-03-22 | 2012-08-01 | 厦门大学 | Method for removing boron-phosphorus impurities from silicon metal |
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