CN103436956A - Quick-melting and slow crystal growth high-efficiency polycrystalline silicon ingot casting process - Google Patents
Quick-melting and slow crystal growth high-efficiency polycrystalline silicon ingot casting process Download PDFInfo
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- CN103436956A CN103436956A CN2013103482745A CN201310348274A CN103436956A CN 103436956 A CN103436956 A CN 103436956A CN 2013103482745 A CN2013103482745 A CN 2013103482745A CN 201310348274 A CN201310348274 A CN 201310348274A CN 103436956 A CN103436956 A CN 103436956A
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- Prior art keywords
- polycrystalline silicon
- ingot
- casting
- melting
- temperature
- Prior art date
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- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 58
- 238000005266 casting Methods 0.000 title claims abstract description 47
- 238000002844 melting Methods 0.000 title claims abstract description 16
- 230000012010 growth Effects 0.000 title abstract description 6
- 238000000034 method Methods 0.000 claims abstract description 33
- XKRFYHLGVUSROY-UHFFFAOYSA-N argon Chemical compound data:image/svg+xml;base64,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 data:image/svg+xml;base64,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 [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000007789 gas Substances 0.000 claims abstract description 19
- 229910052904 quartz Inorganic materials 0.000 claims abstract description 18
- 239000010453 quartz Substances 0.000 claims abstract description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials 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O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000001816 cooling Methods 0.000 claims abstract description 12
- 229910052786 argon Inorganic materials 0.000 claims abstract description 11
- 238000000137 annealing Methods 0.000 claims abstract description 8
- 238000010257 thawing Methods 0.000 claims description 12
- 238000004321 preservation Methods 0.000 claims description 10
- 239000002210 silicon-based material Substances 0.000 claims description 6
- 238000009412 basement excavation Methods 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 230000001934 delay Effects 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- 230000003698 anagen phase Effects 0.000 abstract 3
- 230000000903 blocking Effects 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 230000005611 electricity Effects 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N silicon Chemical compound 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- 229910000077 silane Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
Abstract
The invention belongs to the field of polycrystalline silicon cast ingots and particularly relates to a quick-melting and slow crystal growth high-efficiency polycrystalline silicon ingot casting process. The quick-melting and slow crystal growth high-efficiency polycrystalline silicon ingot casting process comprises the steps of loading, vacuumizing and preheating, melting and preserving heat, growing the crystal, annealing, cooling and blocking, wherein the melting and heat preserving phase and the crystal growing phase are carried out according to the following steps: introducing argon gas into an ingot casting furnace to be used as shielding gas; then heating and raising temperature to enable the temperature of a quartz crucible to reach 1545-1560 DEG C within 4-5 hours, and preserving heat for 7-8 hours; reducing the temperature to 1440 DEG C after 0.5 hour; reducing the temperature of the quartz crucible from 1440 DEG C to 1420 DEG C through 29 hours and finishing the central crystal growing phase of the polycrystalline silicon cast ingot; reducing the temperature to 1410 DEG C after 3 hours to finish the corner crystal growing phase of the polycrystalline silicon cast ingot. The quick-melting and slow crystal growth high-efficiency polycrystalline silicon ingot casting process disclosed by the invention has the advantages that firstly, the photoelectric conversion efficiency of a solar cell can be improved from 17.1 percent to 17.4 percent; secondly, the time of the whole process is shortened while the quality of the polycrystalline silicon cast ingot is improved.
Description
Technical field
The invention belongs to the polycrystalline silicon ingot casting field, be specifically related to the slow long brilliant efficient polycrystalline silicon casting ingot process of a kind of fast thawing.
Background technology
At present, China has become world energy sources production and consumption big country, but the energy expenditure level is also very low per capita.Along with economical and social development, China's energy demand is by sustainable growth, for current energy shortage situation, deep thinking is all being carried out in countries in the world, and effort improves efficiency of energy utilization, promote the development and application of renewable energy source, reduce the dependence to Imported oil, strengthen energy security.
Solar energy power generating development in recent years as one of important development direction of renewable energy source is swift and violent, and its proportion is increasing.According to " planning of renewable energy source Long-and Medium-term Development ", to the year two thousand twenty, China strives making the solar electrical energy generation installed capacity to reach the 1.8GW(gigawatt), will reach 600GW to the year two thousand fifty.Expect the year two thousand fifty, the electric power installation of Chinese renewable energy source will account for 25% of national electric power installation, and wherein the photovoltaic generation installation will account for 5%.Before estimating the year two thousand thirty, the compound growth rate of Chinese sun power installed capacity will be up to more than 25%.
The development of photovoltaic industry depends on the purification to polycrystalline silicon raw material.The purifying technique of polycrystalline silicon raw material is several technique below main the dependence at present: Siemens Method, silane thermal decomposition process, gas fluidized bed method and metallurgy method.Above several method all can relate to the final casting ingot process of polysilicon, and the ingot casting process mainly is divided into six stages, comprises that charging vacuumizes and preheating, melting and heat preservation, long crystalline substance, annealing, cooling and evolution.
At present, the electricity conversion of polysilicon solar battery slice is not also very high, the electricity conversion of the polysilicon solar cell that existing technique obtains is 17.1%, and this makes cost for solar power generation still very high, can not meet the requirement of people for solar electrical energy generation.Therefore, how under existence conditions, by changing the electricity conversion that existing polycrystalline silicon casting ingot process improves solar battery sheet, become a kind of research direction.
Summary of the invention
According to above the deficiencies in the prior art, the present invention proposes the slow long brilliant efficient polycrystalline silicon casting ingot process of a kind of fast thawing, by adjusting the polycrystalline silicon casting ingot process parameter, optimized process flow, reasonably distribute heat fused and long brilliant process time, thereby obtain having the efficient polycrystalline silicon ingot casting of high electricity conversion.
The slow long brilliant efficient polycrystalline silicon casting ingot process of a kind of fast thawing of the present invention, comprise that charging vacuumizes and preheating, melting and heat preservation, long crystalline substance, annealing, cooling and evolution, and wherein, melting and heat preservation and long brilliant stage carry out according to following steps:
(1) melting and heat preservation: to passing into argon gas in ingot furnace as protection gas, heat temperature raising then, make in quartz crucible temperature reach 1545～1560 ℃ and be incubated 7～8h in 4～5h, then through 0.5h, cools to 1440 ℃;
(2) long brilliant: in quartz crucible, temperature is reduced to 1420 ℃ from 1440 ℃ through 29h, completes the brilliant stage of central authorities head of polycrystalline silicon ingot casting, then cools to 1410 ℃ of long brilliant stages of corner that complete polycrystalline silicon ingot casting through 3h.
Wherein, described charging vacuumize and the preheating preferred version as follows: in the quartz crucible that polycrystalline silicon material is packed in ingot furnace, then be evacuated to 0.8～1Pa, open preheating, in 2～3h, in quartz crucible, temperature reaches 1000～1175 ℃.
The purity of described polycrystalline silicon material is preferably 5～6N(99.999%～99.9999%).
Described annealing preferred version is as follows: polycrystalline silicon ingot casting is incubated to 2～4h at 1300～1370 ℃.
Described cooling preferred version is as follows: cooling to passing into the circulation argon gas in ingot furnace, controlling rate of temperature fall is 60～80 ℃/h, takes out polycrystalline silicon ingot casting after being down to 400 ℃.
Described evolution preferred version is as follows: polycrystalline silicon ingot casting is adopted to the excavation machine evolution.
Described in step (1) to passing into argon gas in ingot furnace as protection gas, preferably make furnace pressure remain on 40～60KPa.
In technique of the present invention, the melting and heat preservation time only has 11～13h, and this stage about 17～18h often in existing technique, this technique has shortened the time in this stage greatly, can effectively shorten the ingot casting production cycle, enhances productivity; This technique is in the long brilliant stage, be total to 32h consuming time, extended 1h than this stage in existing technique, this makes long brilliant process liquid-solid interface more steady, be easier to obtain being orientated columanar structure consistent, size uniform, simultaneously, the brilliant process of slower length can also be eliminated the unrelieved stress of inside ingot, reduces dislocation desity.This technique can improve the quality of polycrystalline silicon ingot casting greatly, and the photoelectric transformation efficiency of the cell piece that makes machining obtain obviously improves.
The invention has the advantages that: (1) delays long brilliant technique by fast thawing, and the photoelectric transformation efficiency of solar battery sheet can bring up to 17.4% from 17.1%; (2), when the polycrystalline silicon ingot casting quality improves, shortened the time of whole technique.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.
Embodiment 1:
Carry out polycrystalline silicon casting ingot process according to following steps:
(1) charging vacuumizes and preheating: in the quartz crucible that the polycrystalline silicon material that is 5N by purity is packed in ingot furnace, then be evacuated to 0.8Pa, open preheating, in 2h, in quartz crucible, temperature reaches 1050 ℃.
(2) melting and heat preservation: to passing into argon gas in ingot furnace as protection gas, make furnace pressure remain on 45KPa, heat temperature raising then, make in quartz crucible temperature reach 1545 ℃ and be incubated 7h in 4h, then through 0.5h, cools to 1440 ℃;
(3) long brilliant: in quartz crucible, temperature is reduced to 1420 ℃ from 1440 ℃ through 29h, completes the brilliant stage of central authorities head of polycrystalline silicon ingot casting, then cools to 1410 ℃ of long brilliant stages of corner that complete polycrystalline silicon ingot casting through 3h.
(4) annealing: polycrystalline silicon ingot casting is at 1320 ℃ of insulation 2.5h.
(5) cooling: cooling to passing into the circulation argon gas in ingot furnace, controlling rate of temperature fall is 60 ℃/h, takes out polycrystalline silicon ingot casting after being down to 400 ℃.
(6) evolution: polycrystalline silicon ingot casting is adopted to the excavation machine evolution, obtain little silicon ingot.
(7) little silicon ingot processing is become to cell piece, its electricity conversion is 17.41% after tested.
Embodiment 2:
Carry out polycrystalline silicon casting ingot process according to following steps:
(1) charging vacuumizes and preheating: in the quartz crucible that the polycrystalline silicon material that is 6N by purity is packed in ingot furnace, then be evacuated to 1Pa, open preheating, in 3h, in quartz crucible, temperature reaches 1150 ℃.
(2) melting and heat preservation: to passing into argon gas in ingot furnace as protection gas, make furnace pressure remain on 60KPa, heat temperature raising then, make in quartz crucible temperature reach 1560 ℃ and be incubated 8h in 5h, then through 0.5h, cools to 1440 ℃;
(3) long brilliant: in quartz crucible, temperature is reduced to 1420 ℃ from 1440 ℃ through 29h, completes the brilliant stage of central authorities head of polycrystalline silicon ingot casting, then cools to 1410 ℃ of long brilliant stages of corner that complete polycrystalline silicon ingot casting through 3h.
(4) annealing: polycrystalline silicon ingot casting is at 1370 ℃ of insulation 4h.
(5) cooling: cooling to passing into the circulation argon gas in ingot furnace, controlling rate of temperature fall is 80 ℃/h, takes out polycrystalline silicon ingot casting after being down to 400 ℃.
(6) evolution: polycrystalline silicon ingot casting is adopted to the excavation machine evolution, obtain little silicon ingot.
(7) little silicon ingot processing is become to cell piece, its electricity conversion is 17.44% after tested.
Claims (7)
1. the slow long brilliant efficient polycrystalline silicon casting ingot process of a fast thawing, comprising that charging vacuumizes and preheating, melting and heat preservation, long crystalline substance, annealing, cooling and evolution, it is characterized in that melting and heat preservation and long crystalline substance stage carry out according to following steps:
(1) melting and heat preservation: to passing into argon gas in ingot furnace as protection gas, heat temperature raising then, make in quartz crucible temperature reach 1545～1560 ℃ and be incubated 7～8h in 4～5h, then through 0.5h, cools to 1440 ℃;
(2) long brilliant: in quartz crucible, temperature is reduced to 1420 ℃ from 1440 ℃ through 29h, completes the brilliant stage of central authorities head of polycrystalline silicon ingot casting, then cools to 1410 ℃ of long brilliant stages of corner that complete polycrystalline silicon ingot casting through 3h.
2. fast thawing according to claim 1 delays long brilliant efficient polycrystalline silicon casting ingot process, it is characterized in that described charging vacuumizes and preheating is in the quartz crucible that polycrystalline silicon material is packed in ingot furnace, then be evacuated to 0.8～1Pa, open preheating, in 2～3h, in quartz crucible, temperature reaches 1000～1175 ℃.
3. fast thawing according to claim 2 delays long brilliant efficient polycrystalline silicon casting ingot process, and the purity that it is characterized in that described polycrystalline silicon material is 5～6N.
4. the slow long brilliant efficient polycrystalline silicon casting ingot process of fast thawing according to claim 1, is characterized in that described annealing is at 1300～1370 ℃ of insulation 2～4h by polycrystalline silicon ingot casting.
5. the slow long brilliant efficient polycrystalline silicon casting ingot process of fast thawing according to claim 1, is characterized in that described cooling is that to pass into the circulation argon gas in ingot furnace cooling, and controlling rate of temperature fall is 60～80 ℃/h, takes out polycrystalline silicon ingot casting after being down to 400 ℃.
6. the slow long brilliant efficient polycrystalline silicon casting ingot process of fast thawing according to claim 1, is characterized in that described evolution is that polycrystalline silicon ingot casting is adopted to the excavation machine evolution.
7. the slow long brilliant efficient polycrystalline silicon casting ingot process of fast thawing according to claim 1, is characterized in that passing into argon gas as protection gas described in step (1) in ingot furnace, makes furnace pressure remain on 40～60KPa.
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