CN103436957A - Polycrystalline silicon ingot casting process with double-mode control on melting and heat insulation - Google Patents

Polycrystalline silicon ingot casting process with double-mode control on melting and heat insulation Download PDF

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Publication number
CN103436957A
CN103436957A CN2013103741364A CN201310374136A CN103436957A CN 103436957 A CN103436957 A CN 103436957A CN 2013103741364 A CN2013103741364 A CN 2013103741364A CN 201310374136 A CN201310374136 A CN 201310374136A CN 103436957 A CN103436957 A CN 103436957A
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China
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polycrystalline silicon
ingot
melting
temperature
casting
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CN2013103741364A
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Inventor
李鹏廷
王峰
安广野
姜大川
熊华江
黄佳琪
谭毅
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Qingdao Longsheng Crystalline Silicon Science & Technology Co Ltd
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Qingdao Longsheng Crystalline Silicon Science & Technology Co Ltd
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Priority to CN2013103741364A priority Critical patent/CN103436957A/en
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Abstract

The invention belongs to polycrystalline silicon ingot casting processes, and particularly relates to a polycrystalline silicon ingot casting process with double-mode control on melting and heat insulation. The polycrystalline silicon ingot casting process comprises the steps of charging and vacuumizing, melting and heat insulation, crystal growth, annealing, cooling and ingot cutting, and is characterized in that in the phase of melting and heat insulation, a power control mode is used and a temperature in a quartz crucible is caused to achieve a melting temperature by increasing the power of a heater at first, and then a temperature control mode is used and the melting temperature is controlled to be invariable to perform heat insulation. The polycrystalline silicon ingot casting process disclosed by the invention has the following advantages that (1) a temperature for controlling mode conversion is the melting temperature, thus omitting the step of preheating and then heating, and in addition, heating is realized by a high power at first, thus reducing the time of the whole process by 3-4 hours; (2) due to the reduction for the time of the process, the cost of the whole ingot casting process can be reduced by about 5%.

Description

The polycrystalline silicon casting ingot process of double mode controlled melting insulation
Technical field
The invention belongs to polycrystalline silicon casting ingot process, be specifically related to a kind of polycrystalline silicon casting ingot process of double mode controlled melting insulation.
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, comprising that charging vacuumizes, 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 is unfavorable for the development of solar energy industry.Wherein, existing casting ingot process needs 60~65 hours, and wherein the melting and heat preservation stage has just occupied very large ratio, about 18~20h.Reason mainly contains 2 points, and the one, can't directly by temperature, control, the fusing point of silicon is higher, sets the comparatively high temps parameter and easily makes the well heater overwork, increases the well heater burden; The 2nd, need long preheating in prior art, preheating is carried out under lower power, then reaches a lower preheating temperature and starts conversion temp control, is warming up to temperature of fusion insulation.
Summary of the invention
According to above the deficiencies in the prior art, the polycrystalline silicon casting ingot process that the purpose of this invention is to provide a kind of double mode controlled melting insulation, by the technique adjustment, adopt power and two kinds of pattern controlled melting holding stages of temperature, accelerate heating and burn-off rate, realize shortening the purpose in ingot casting cycle.
The polycrystalline silicon casting ingot process of a kind of double mode controlled melting insulation of the present invention, comprising that charging vacuumizes, melting and heat preservation, long crystalline substance, annealing, cooling and evolution, melting and heat preservation is in the stage, first adopt power control mode, by increasing heater power, make temperature in quartz crucible reach temperature of fusion, then adopt temp-controled mode, controlled melting is temperature-resistant to be incubated.
The melting and heat preservation stage preferably carries out successively according to following steps:
(1) adopt power control mode: pass into argon gas as protection gas, making pressure in ingot furnace is 40~60KPa, and in 1~1.5h, heating power is increased to 85% by 10%, then in 2~3h, makes temperature in quartz crucible reach 1560~1580 ℃;
(2) adopt temp-controled mode: in 1560~1580 ℃ of scopes, be incubated 7~8h.
Wherein, it is as follows that described charging vacuumizes preferred version: in the quartz crucible that polycrystalline silicon material is packed in ingot furnace, then be evacuated to 0.6~1.0Pa.
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.
The brilliant preferred version of described length is as follows: after insulation finishes, first will in ingot furnace, by passing into argon gas, make pressure be adjusted to 50~70KPa, cool to 1440 ℃ through 0.5h, then cool to 1420 ℃ through 25~27h, complete the long brilliant stage of central authorities, then cool to 1410 ℃ through 2~3h and complete 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, do not need preheating, directly by power control mode, reach at short notice temperature of fusion, more constant in the temperature of fusion scope by temp-controled mode, be incubated.Owing to having omitted pre-heating step, so the process time shortening.
The invention has the advantages that: the temperature of (1) master mode conversion is temperature of fusion, has saved the step that preheating heats up again, by superpower, heats at the beginning in addition, has shortened the time 3~4h of whole technique; (2), due to the shortening of process time, can make the cost about 5% of whole casting ingot process.
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: in the quartz crucible that the polycrystalline silicon material 650kg that is 5N by purity packs in ingot furnace, then be evacuated to 0.6Pa.
(2) melting and heat preservation: first adopt power control mode, pass into argon gas as protection gas, making pressure in ingot furnace is 40KPa, and total power is 168kw, and in 1h, heating power is increased to 85% by 10%, then in 2h, makes temperature in quartz crucible reach 1560 ℃; Adopt again temp-controled mode: at 1560 ℃ of insulation 7h.
(3) it is long brilliant: after insulation finishes, first, by ingot furnace, by passing into argon gas, making pressure be adjusted to 50KPa, through 0.5h, cool to 1440 ℃, then through 25h, cool to 1420 ℃, complete the long brilliant stage of central authorities, then cool to 1410 ℃ through 2h and complete the long brilliant stage of corner.
(4) annealing: polycrystalline silicon ingot casting is cooled in 0.5h to 1310 ℃ and be incubated 2h.
(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, after excision top impurity and surrounding corner material, is placed in to excavation machine and carries out evolution.
Embodiment 2:
Carry out polycrystalline silicon casting ingot process according to following steps:
(1) charging vacuumizes: in the quartz crucible that the polycrystalline silicon material 650kg that is 6N by purity packs in ingot furnace, then be evacuated to 1.0Pa.
(2) melting and heat preservation: first adopt power control mode, pass into argon gas as protection gas, making pressure in ingot furnace is 60KPa, and total power is 168kw, in 1.5h, heating power is increased to 85% by 10%, then in 3h, makes temperature in quartz crucible reach 1580 ℃; Adopt again temp-controled mode: at 1580 ℃ of insulation 8h.
(3) it is long brilliant: after insulation finishes, first, by ingot furnace, by passing into argon gas, making pressure be adjusted to 70KPa, through 0.5h, cool to 1440 ℃, then through 27h, cool to 1420 ℃, complete the long brilliant stage of central authorities, then cool to 1410 ℃ through 3h and complete the long brilliant stage of corner.
(4) annealing: polycrystalline silicon ingot casting is cooled in 0.5h to 1370 ℃ and be incubated 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, after excision top impurity and surrounding corner material, is placed in to excavation machine and carries out evolution.

Claims (8)

1. the polycrystalline silicon casting ingot process of a double mode controlled melting insulation, comprising that charging vacuumizes, melting and heat preservation, long crystalline substance, annealing, cooling and evolution, it is characterized in that melting and heat preservation is in the stage, first adopt power control mode, by increasing heater power, make temperature in quartz crucible reach temperature of fusion, then adopt temp-controled mode, controlled melting is temperature-resistant to be incubated.
2. the polycrystalline silicon casting ingot process of double mode controlled melting insulation according to claim 1 is characterized in that the melting and heat preservation stage carries out successively according to following steps:
(1) adopt power control mode: pass into argon gas as protection gas, making pressure in ingot furnace is 40~60KPa, and in 1~1.5h, heating power is increased to 85% by 10%, then in 2~3h, makes temperature in quartz crucible reach 1560~1580 ℃;
(2) adopt temp-controled mode: in 1560~1580 ℃ of scopes, be incubated 7~8h.
3. the polycrystalline silicon casting ingot process of double mode controlled melting insulation according to claim 1, is characterized in that it is in the quartz crucible that polycrystalline silicon material is packed in ingot furnace that described charging vacuumizes, and then is evacuated to 0.6~1.0Pa.
4. the polycrystalline silicon casting ingot process that double mode controlled melting according to claim 3 is incubated, the purity that it is characterized in that described polycrystalline silicon material is 5~6N.
5. the polycrystalline silicon casting ingot process that double mode controlled melting according to claim 1 is incubated, it is characterized in that described long crystalline substance is after insulation finishes, first will in ingot furnace, by passing into argon gas, make pressure be adjusted to 50~70KPa, cool to 1440 ℃ through 0.5h, then cool to 1420 ℃ through 25~27h, complete the long brilliant stage of central authorities, then cool to 1410 ℃ through 2~3h and complete the long brilliant stage of corner.
6. the polycrystalline silicon casting ingot process of double mode controlled melting insulation according to claim 1, 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.
7. the polycrystalline silicon casting ingot process of double mode controlled melting insulation 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 ℃.
8. the polycrystalline silicon casting ingot process of double mode controlled melting insulation according to claim 1, 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.
CN2013103741364A 2013-08-23 2013-08-23 Polycrystalline silicon ingot casting process with double-mode control on melting and heat insulation Pending CN103436957A (en)

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Cited By (4)

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Publication number Priority date Publication date Assignee Title
CN103882518A (en) * 2014-03-28 2014-06-25 大连理工大学 Polycrystalline silicon ingot casting process achieving uniform distribution of boron
CN106087043A (en) * 2016-08-10 2016-11-09 中联西北工程设计研究院有限公司 A kind of polysilicon fritting casting ingot method and device
CN106435728A (en) * 2016-09-23 2017-02-22 江苏美科硅能源有限公司 Crystal growing process for ingot casting in polycrystalline furnace
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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CN103205797A (en) * 2012-01-17 2013-07-17 北京京运通科技股份有限公司 High-efficiency polycrystalline silicon ingot casting method
CN103215633A (en) * 2013-04-10 2013-07-24 衡水英利新能源有限公司 Method for casting ingots by polycrystalline silicon

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CN101864594A (en) * 2010-06-10 2010-10-20 晶海洋半导体材料(东海)有限公司 Ingot casting method for quasi-monocrystalline silicon
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103882518A (en) * 2014-03-28 2014-06-25 大连理工大学 Polycrystalline silicon ingot casting process achieving uniform distribution of boron
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CN106435728A (en) * 2016-09-23 2017-02-22 江苏美科硅能源有限公司 Crystal growing process for ingot casting in polycrystalline furnace
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: 20131211