CN103469302A - Polycrystalline silicon ingoting process for shortening corner crystal growth time - Google Patents
Polycrystalline silicon ingoting process for shortening corner crystal growth time Download PDFInfo
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- CN103469302A CN103469302A CN2013103734873A CN201310373487A CN103469302A CN 103469302 A CN103469302 A CN 103469302A CN 2013103734873 A CN2013103734873 A CN 2013103734873A CN 201310373487 A CN201310373487 A CN 201310373487A CN 103469302 A CN103469302 A CN 103469302A
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- polycrystalline silicon
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- long brilliant
- ingoting
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- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 35
- 238000004904 shortening Methods 0.000 title claims abstract description 15
- 239000013078 crystal Substances 0.000 title abstract description 9
- 238000000137 annealing Methods 0.000 claims abstract description 14
- 239000012535 impurity Substances 0.000 claims abstract description 8
- 238000002844 melting Methods 0.000 claims abstract description 8
- 230000008018 melting Effects 0.000 claims abstract description 8
- 238000005266 casting Methods 0.000 claims description 37
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 239000010453 quartz Substances 0.000 claims description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 16
- 239000007789 gas Substances 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 11
- 239000000126 substance Substances 0.000 claims description 9
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 238000004321 preservation Methods 0.000 claims description 7
- 239000002210 silicon-based material Substances 0.000 claims description 7
- 238000009412 basement excavation Methods 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 238000009792 diffusion process Methods 0.000 abstract description 3
- 238000005086 pumping Methods 0.000 abstract 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 238000009434 installation Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 239000012467 final product Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 238000010248 power generation Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 210000002615 epidermis Anatomy 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
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- Silicon Compounds (AREA)
Abstract
The invention belongs to the field of polycrystalline silicon ingoting, and particularly relates to a polycrystalline silicon ingoting process for shortening corner crystal growth time. The process comprises the following steps: loading, vacuum-pumping, preheating, melting and heat-insulating, crystal growth, annealing, temperature reduction and squaring, wherein the step of crystal growth comprises a central crystal growth stage and a corner crystal growth stage. The polycrystalline silicon ingoting process is characterized in that the next step of annealing stage can be performed after 1/4-1/6 of the corner crystal growth stage is completed. The ingoting process has the advantages as follows: 1, through shortening the time of the corner crystal growth stage, the annealing stage comes in advance, and the whole process time is effectively shortened by 2-3 h, and moreover, back diffusion of impurities at the ingoting top can be effectively prevented so as to improve the polycrystalline silicon ingoting quality; 2, as the process time is shortened, the expenditure on electric power and manual labour is reduced, and as a result, the cost of the whole ingoting process is reduced by 5 percent.
Description
Technical field
The invention belongs to the polycrystalline silicon ingot casting field, be specifically related to a kind of corner polycrystalline silicon casting ingot process of long brilliant time that shortens.
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.
In the long brilliant stage, start to solidify long crystalline substance bottom silicon liquid, because long crystal boundary face is convex, so central part can first solidify the long brilliant silicon liquid upper surface that arrives, complete the brilliant stage of central authorities' length; Then the both sides, top more slowly long crystalline substance complete, complete the long brilliant stage of corner.At present, it is still very high that cost for solar power generation is compared thermal power generation, and this makes how to reduce costs a direction that becomes research.Wherein, in the long brilliant stage used time very long, generally need more than 60 hours, this makes the costs such as manpower in the ingot casting process, electric power high.Therefore, shortening as far as possible the ingot casting cycle is very important.
Summary of the invention
According to above the deficiencies in the prior art, the objective of the invention is to propose a kind of corner polycrystalline silicon casting ingot process of long brilliant time that shortens, by shortening the long brilliant time of corner, to reach, save manpower and power cost, reduce the cost of solar electrical energy generation with this.
A kind of corner polycrystalline silicon casting ingot process of long brilliant time that shortens of the present invention, comprise that charging vacuumizes and preheating, melting and heat preservation, long crystalline substance, annealing, cooling and evolution, wherein, long crystalline substance comprises long brilliant stage of central authorities and long brilliant stage of corner, and the long brilliant stage of corner proceeds at 1/4～1/6 o'clock and carries out next step annealing stage.
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 0.5～0.9Pa, open preheating, in 2～3h, in quartz crucible, temperature reaches 1100～1200 ℃.
The purity of described polycrystalline silicon material is preferably 5～6N(99.999%～99.9999%).The polycrystalline silicon ingot casting stage requires the purity of silicon material to want high, for solar cell, usually requires at 5～6N, as long as therefore meet this requirement.
Described melting and heat preservation preferred version is as follows: to passing into argon gas in ingot furnace as protection gas, make furnace pressure remain on 40～60KPa, heat temperature raising then, make in quartz crucible temperature reach 1550～1570 ℃ and be incubated 8～9h in 4～6h.
The long brilliant stage preferred version of described central authorities is as follows: first furnace pressure is adjusted to 50～70KPa, then in 0.5h, temperature in quartz crucible is dropped to 1420～1430 ℃, then temperature is reduced to 1410～1415 ℃ from 1420～1430 ℃ through 27～29h.
The long brilliant stage preferred version in described corner is as follows: cool to 1405～1410 ℃ at 0.5h, complete 1/4～1/6 of the long brilliant stage of corner.
Described annealing preferred version is as follows: polycrystalline silicon ingot casting is cooled in 0.5h to 1310～1370 ℃ and be incubated 2～4h.
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, after excision top impurity and surrounding corner material, is placed in to excavation machine and carries out evolution.
In technique of the present invention, the long brilliant stage of corner gets final product while only proceeding to 1/4～1/6 degree, do not need remainder all long crystalline substance complete.Major cause is in the polycrystalline silicon ingot casting process, impurity wherein is subject to the meeting that affects of segregation coefficient and concentrates and solidify at upper epidermis, therefore after ingot casting completes, need excision silicon ingot top 3～4cm, and the thickness in long brilliant stage of corner is also 3～4cm, so fundamentally do not need the long crystalline substance in corner to complete, only need in follow-up annealing process, solidify and get final product.And only proceed to 1/4～1/6 stage, be to consider for the back diffusion of top impurity.
The invention has the advantages that: (1), by shortening the corner time in long brilliant stage, enters annealing stage in advance, has effectively shortened whole process time 2～3h, and can also effectively prevent the back diffusion of ingot casting top impurity, improves the quality of polycrystalline silicon ingot casting; (2) due to the shortening of process time, reduced the expenditure of electric power and human cost, make cost 5% left and right of whole casting ingot process.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.
Embodiment 1:
Carry out polycrystalline silicon ingot casting according to following technique:
(1) charging vacuumizes and preheating: be in the 5N polycrystalline silicon material quartz crucible of packing in ingot furnace by purity, then be evacuated to 0.5Pa, open preheating, in 2h, in quartz crucible, temperature reaches 1100 ℃.
(2) melting and heat preservation: to passing into argon gas in ingot furnace as protection gas, make furnace pressure remain on 40KPa, heat temperature raising then, make in quartz crucible temperature reach 1550 ℃ and be incubated 8h in 4h.
(3) the long brilliant stage of central authorities: first furnace pressure is adjusted to 50KPa, then in 0.5h, temperature in quartz crucible is dropped to 1420 ℃, then temperature is reduced to 1410 ℃ from 1420 ℃ through 27h.
(4) the long brilliant stage of corner: cool to 1405 ℃ at 0.5h, complete 1/6 of the long brilliant stage of corner.
(5) annealing: polycrystalline silicon ingot casting is cooled in 0.5h to 1310 ℃ and be incubated 2h.
(6) 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 ℃.
(7) evolution: polycrystalline silicon ingot casting, after excision top impurity and surrounding corner material, is placed in to excavation machine and carries out evolution.
Embodiment 2:
(1) charging vacuumizes and preheating: be in the 6N polycrystalline silicon material quartz crucible of packing in ingot furnace by purity, then be evacuated to 0.9Pa, open preheating, in 3h, in quartz crucible, temperature reaches 1200 ℃.
(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 1570 ℃ and be incubated 9h in 6h.
(3) the long brilliant stage of central authorities: first furnace pressure is adjusted to 70KPa, then in 0.5h, temperature in quartz crucible is dropped to 1430 ℃, then temperature is reduced to 1415 ℃ from 1430 ℃ through 29h.
(4) the long brilliant stage of corner: cool to 1410 ℃ at 0.5h, complete 1/4 of the long brilliant stage of corner.
(5) annealing: polycrystalline silicon ingot casting is cooled in 0.5h to 1370 ℃ and be incubated 4h.
(6) 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 ℃.
(7) evolution: polycrystalline silicon ingot casting, after excision top impurity and surrounding corner material, is placed in to excavation machine and carries out evolution.
Claims (9)
1. one kind is shortened the corner polycrystalline silicon casting ingot process of long brilliant time, comprise that charging vacuumizes and preheating, melting and heat preservation, long crystalline substance, annealing, cooling and evolution, wherein, long crystalline substance comprises long brilliant stage of central authorities and long brilliant stage of corner, it is characterized in that the long brilliant stage of corner proceeds at 1/4～1/6 o'clock and carries out next step annealing stage.
2. the polycrystalline silicon casting ingot process of brilliant time is grown in shortening according to claim 1 corner, 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 0.5～0.9Pa, open preheating, in 2～3h, in quartz crucible, temperature reaches 1100～1200 ℃.
3. the polycrystalline silicon casting ingot process of brilliant time is grown in shortening according to claim 2 corner, and the purity that it is characterized in that described polycrystalline silicon material is 5～6N.
4. the polycrystalline silicon casting ingot process of brilliant time is grown in shortening according to claim 1 corner; it is characterized in that described melting and heat preservation is to pass into argon gas as protection gas in ingot furnace; make furnace pressure remain on 40～60KPa; then heat temperature raising, make in quartz crucible temperature reach 1550～1570 ℃ and be incubated 8～9h in 4～6h.
5. the polycrystalline silicon casting ingot process of brilliant time is grown in shortening according to claim 1 corner, it is characterized in that described central authorities are first furnace pressure to be adjusted to 50～70KPa in the long brilliant stage, then in 0.5h, temperature in quartz crucible is dropped to 1420～1430 ℃, then temperature is reduced to 1410～1415 ℃ from 1420～1430 ℃ through 27～29h.
6. the polycrystalline silicon casting ingot process of long brilliant time of shortening according to claim 1 corner, is characterized in that the long brilliant stage of described corner is to cool to 1405～1410 ℃ at 0.5h, completes 1/4～1/6 of the long brilliant stage of corner.
7. the polycrystalline silicon casting ingot process of long brilliant time of shortening according to claim 1 corner, is characterized in that described annealing is polycrystalline silicon ingot casting to be cooled in 0.5h to 1310～1370 ℃ and be incubated 2～4h.
8. the polycrystalline silicon casting ingot process of long brilliant time of shortening according to claim 1 corner, 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 ℃.
9. the polycrystalline silicon casting ingot process of long brilliant time of shortening according to claim 1 corner, it is characterized in that described evolution be by polycrystalline silicon ingot casting after excision top impurity and surrounding corner material, be placed in excavation machine and carry out evolution.
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| CN2013103734873A CN103469302A (en) | 2013-08-23 | 2013-08-23 | Polycrystalline silicon ingoting process for shortening corner crystal growth time |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104480526A (en) * | 2014-12-04 | 2015-04-01 | 青岛隆盛晶硅科技有限公司 | Preparation method of high-borosilicate material |
| CN105220227A (en) * | 2015-10-27 | 2016-01-06 | 天津英利新能源有限公司 | A kind of efficient polycrystalline silicon casting ingot process |
| CN106087041A (en) * | 2016-06-17 | 2016-11-09 | 江西赛维Ldk太阳能高科技有限公司 | A kind of method removing polysilicon impurity during ingot casting |
| CN108315813A (en) * | 2018-01-04 | 2018-07-24 | 晶科能源有限公司 | A kind of preparation method of polycrystalline silicon ingot casting |
| CN108546989A (en) * | 2018-06-12 | 2018-09-18 | 山东大海新能源发展有限公司 | A kind of preparation process and its polycrystal silicon ingot of polycrystal silicon ingot |
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| CN102409402A (en) * | 2011-11-22 | 2012-04-11 | 江苏金晖光伏有限公司 | Ingot casting process for 650kg polycrystalline silicon |
| CN102925958A (en) * | 2012-08-16 | 2013-02-13 | 江西旭阳雷迪高科技股份有限公司 | Method for improving poly-crystal quality by using re-melting technology |
| CN102978687A (en) * | 2012-12-21 | 2013-03-20 | 英利集团有限公司 | Crystal growth method of polycrystalline silicon ingot |
-
2013
- 2013-08-23 CN CN2013103734873A patent/CN103469302A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102409402A (en) * | 2011-11-22 | 2012-04-11 | 江苏金晖光伏有限公司 | Ingot casting process for 650kg polycrystalline silicon |
| CN102925958A (en) * | 2012-08-16 | 2013-02-13 | 江西旭阳雷迪高科技股份有限公司 | Method for improving poly-crystal quality by using re-melting technology |
| CN102978687A (en) * | 2012-12-21 | 2013-03-20 | 英利集团有限公司 | Crystal growth method of polycrystalline silicon ingot |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104480526A (en) * | 2014-12-04 | 2015-04-01 | 青岛隆盛晶硅科技有限公司 | Preparation method of high-borosilicate material |
| CN105220227A (en) * | 2015-10-27 | 2016-01-06 | 天津英利新能源有限公司 | A kind of efficient polycrystalline silicon casting ingot process |
| CN106087041A (en) * | 2016-06-17 | 2016-11-09 | 江西赛维Ldk太阳能高科技有限公司 | A kind of method removing polysilicon impurity during ingot casting |
| CN106087041B (en) * | 2016-06-17 | 2018-10-26 | 江西赛维Ldk太阳能高科技有限公司 | A kind of method that ingot casting removes polycrystalline silicon impurities in the process |
| CN108315813A (en) * | 2018-01-04 | 2018-07-24 | 晶科能源有限公司 | A kind of preparation method of polycrystalline silicon ingot casting |
| CN108546989A (en) * | 2018-06-12 | 2018-09-18 | 山东大海新能源发展有限公司 | A kind of preparation process and its polycrystal silicon ingot of polycrystal silicon ingot |
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Application publication date: 20131225 |