CN102925972A - Special furnace for casting ingot from impurity silicon and ingot casting method using furnace - Google Patents
Special furnace for casting ingot from impurity silicon and ingot casting method using furnace Download PDFInfo
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- CN102925972A CN102925972A CN2012104260992A CN201210426099A CN102925972A CN 102925972 A CN102925972 A CN 102925972A CN 2012104260992 A CN2012104260992 A CN 2012104260992A CN 201210426099 A CN201210426099 A CN 201210426099A CN 102925972 A CN102925972 A CN 102925972A
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Abstract
The invention discloses a special furnace for casting a polycrystalline silicon ingot from impurity silicon and an ingot casting method using the special furnace. The special furnace for casting the polycrystalline silicon ingot by the impurity silicon comprises a furnace body, a heater covering on a crucible and a heat-insulating cage covering on the heater, wherein the furnace body is provided with a gas inlet and a gas outlet; the furnace body is internally provided with a graphite platform; the crucible is arranged on the graphite platform, and the distance between the top in the heat-insulating cage and the upper surface of the graphite platform is slightly less than the double heights of the crucible. When the polycrystalline silicon ingot is cast from the impurity silicon by using the furnace, the crucible filled with silicon raw material is put on the graphite platform, the furnace body is closed, the furnace body is internally vacuumized, the protective gas is added, the silicon raw material is melted in a heating way, the nucleation is solidified, and the cooling is carried out. The working process shows that after the polycrystalline silicon ingot is cast from the impurity silicon by using the furnace, the production cost can be reduced, the yield of single furnace can be greatly improved, and the quality of the polycrystalline silicon can be greatly improved.
Description
Technical field
The present invention relates to photoelectric field, be specifically related to a kind of assorted material silicon casting polycrystal silicon ingot special furnace and casting ingot method thereof.
Background technology
In the photoelectric field, silicon is raw semiconductor very important and commonly used, is the optimal starting material of solar cell.After the operations such as the silicon raw material generally will pass through cleaning, ingot casting, stripping and slicing, viscose glue, cuts into slices, comes unstuck, cleaning, could be used for solar cell.Because the polycrystal silicon ingot steady quality that ingot casting silicon stove is produced, the casting ingot process comparative maturity now is widely used.But cast polycrystal silicon ingot at this ingot casting silicon stove with assorted material silicon, its utilization ratio is lower, generally can only reach about 60 percent, and single furnace output is also lower, and single stove is not generally all reaching half ton below half ton.Monocrystal silicon waste materials in the monocrystalline silicon production factory manufacture order crystal silicon process that described assorted material silicon refers to reclaim, and the polycrystalline silicon wastes that produces in the polycrystalline silicon ingot casting process.
Summary of the invention
The object of the invention is to: overcome the deficiencies in the prior art, provide a kind of utilization to mix and expect silicon casting polycrystal silicon ingot special furnace and casting ingot method thereof, make casting decide production cost reduction, the raising of polysilicon quality, while ingot casting output also is improved.
The technical solution used in the present invention is:
Assorted material silicon casting polycrystal silicon ingot special furnace, comprise body of heater, described body of heater is provided with inlet mouth and air outlet, be provided with graphite platform in the body of heater, be placed with crucible on the described graphite platform, also comprise cover cap in the well heater of crucible, cover cap is in the heat-insulation cage of well heater, and the distance between described heat-insulation cage inner top and the graphite platform upper surface is slightly less than 2 times of crucible height.
The further improvement project of the present invention is that the internal surface of described crucible scribbles silicon nitride coating.
The present invention further improvement project is, the internal surface in downward 3 ~ 8 cm range of crucible limit mouth scribbles the individual layer silicon nitride coating, and all the other internal surfaces scribble the nitride multilayer silicon coating.
Carry out the method for polycrystalline silicon ingot casting with above-mentioned assorted material silicon casting polycrystal silicon ingot special furnace, may further comprise the steps:
The crucible that 1) will fill raw silicon is positioned over graphite platform, and body of heater is closed;
2) heat-insulation cage is promoted slightly, make between heat-insulation cage bottom and the graphite platform upper surface gappedly, and pass through the air outlet, with vacuum pumping state in the body of heater, body of heater carries out preheating;
3) add protection gas by inlet mouth in body of heater, the air pressure in the body of heater is increased to 600 millibars gradually, heater heats, and is heated to gradually about 1200 degrees centigrade in half an hour, and keeps about half an hour; Again the temperature in the body of heater is heated to about 1550 degrees centigrade, raw silicon is all melted;
4) keeping the body of heater internal gas pressure is 600 millibars, closes well heater, and promotes heat-insulation cage to 1/5th positions of crucible height, makes the drop in temperature in the body of heater and remains on about 1440 degrees centigrade, makes the silicon material of fusing long brilliant;
5) after 2 hours, keeping the body of heater internal gas pressure is 600 millibars, and heat-insulation cage is divided four times, and contour 1/3rd positions that are promoted to the crucible height make temperature in the body of heater from about 1440 degrees centigrade of left and right sides slow decreasings to 1410 degree centigrade;
6) keep the body of heater internal gas pressure and still be 600 millibars, about drop in temperature to 1370 degree centigrade, heat-insulation cage is dropped to graphite platform, and kept this state 3.5 hours in the body of heater, make the silicon ingot annealing behind the long crystalline substance;
7) increase the gas flow of air outlet, inlet mouth, keep the body of heater internal gas pressure and still be 600 millibars, approximately after 3 hours, divide 2/3rds positions that are promoted to the crucible height for three times with heat-insulation cage, make in the body of heater about drop in temperature to 400 degree centigrade;
8) open body of heater, crucible is taken out, and silicon ingot is naturally cooled to room temperature get final product.
The present invention further improvement project is, in the described step 1), comprise polysilicon and silicon single crystal in the raw silicon, the mass ratio of described polysilicon and silicon single crystal is 1:1, described silicon single crystal is as flavoring food, and the silicon single crystal flavoring food need to carry out annealing operation under the temperature about 550 degrees centigrade before ingot casting.
The present invention further improvement project is, in the described step 5), in long brilliant process, the solidification rate of silicon liquid per hour carried out one-time detection.
The present invention further improvement project is that in the described step 5), keep this state 2 ~ 3 hour after the lifting first time, keeps this state about 7 hours after promoting for the second time, keeps this state about 17 hours after promoting for the third time; Keep this state about 4 hours after last the lifting; In the meantime, the temperature in the body of heater is from about 1440 degrees centigrade of left and right sides slow decreasings to 1410 degree centigrade, and the body of heater internal gas pressure is kept 600 millibars.
The present invention further improvement project is, in the described step 7), heat-insulation cage is promoted to 1/4th positions of crucible height for the first time, and body of heater pressure increases to 700 millibars, and keeps this state 2 hours, for the second time promote heat-insulation cage to 1/2nd positions of crucible height, and kept this state 7 ~ 8 hours, and at last heat-insulation cage is promoted to 2/3rds positions of crucible height, close the air outlet, air pressure in the body of heater is forced into 850 millibars, keeps this state about half an hour.
Beneficial effect of the present invention is:
When mixing material silicon casting polycrystal silicon ingot with the present invention, select assorted material silicon, can greatly reduce production costs; The monocrystalline sila material that outsourcing is returned is annealed under 550 degrees centigrade first before ingot casting, and the resistance value of silicon single crystal flavoring food is stablized; Increase the distance between heat-insulation cage and the graphite platform, can make the temperature in the heat-insulation cage more stable, temperature variation more relaxes, and is conducive to the long brilliant of silicon material; Because after the fusing of silicon raw material, there is certain distance on silicon liquid surface with crucible limit mouth, can save certain cost so be coated with the individual layer silicon nitride coating in downward 3 ~ 8 cm range of crucible limit mouth; With the brilliant time lengthening of the length of silicon material, and in the brilliant process of the length of silicon material, per hour all once monitor, guarantee that the brilliant speed of length of silicon material is in optimum regime.Hence one can see that, with the present invention's material silicon casting polycrystal silicon ingot of mixing, not only can reduce production costs, only increase under the condition of ten Percent in single stove energy consumption, single furnace output has improved 35 percent, and greatly improved the quality of polycrystal silicon ingot, make the utilization ratio of polycrystal silicon ingot improve ten Percent.
Description of drawings
Fig. 1 is schematic flow sheet of the present invention.
Fig. 2 is that structure master of the present invention looks cross-sectional schematic.
Embodiment
As shown in Figure 1, the present invention includes body of heater 1, described body of heater 1 is provided with inlet mouth 4 and air outlet 5, be provided with graphite platform 3 in the body of heater 1, be placed with on the described graphite platform 3 in the crucible 7(the implementation case, the model of crucible 7 is 540 types), comprise that also cover cap is in the well heater 8 of crucible 7, cover cap is in the heat-insulation cage 2 of well heater 8, and the distance between described heat-insulation cage 2 inner tops and graphite platform 3 upper surfaces is slightly less than 2 times of crucible 7 height; The internal surface of described crucible 7 scribbles silicon nitride coating 9; Internal surface in downward 3 ~ 8 cm range of crucible 7 limit mouths scribbles in the individual layer silicon nitride coating 9(the implementation case, apart from scribbling individual layer silicon nitride coating 9 in crucible 7 Open Side Down 5 centimetres the scope), all the other internal surfaces scribble nitride multilayer silicon coating 9.
Carry out the method for polycrystalline silicon ingot casting with the present invention, may further comprise the steps:
The crucible 7 that will fill first raw silicon 6 is positioned over graphite platform 3, and with body of heater 1 closure; Comprise polysilicon and silicon single crystal in the described raw silicon 6, the mass ratio of described polysilicon and silicon single crystal is 1:1, and described silicon single crystal is as flavoring food, and the silicon single crystal flavoring food need to carry out annealing operation under the temperature about 550 degrees centigrade before ingot casting; Heat-insulation cage 2 is promoted slightly again, make between heat-insulation cage 2 bottoms and graphite platform 3 upper surfaces gappedly, and by air outlet 5, with body of heater 1 interior vacuum pumping state, body of heater 1 carries out preheating; To body of heater 1 interior adding protection gas, the air pressure in the body of heater 1 is increased to gradually 600 millibars by inlet mouth 4, heater 8 heats, and is heated to gradually about 1200 degrees centigrade in half an hour, and keeps about half an hour; Again the temperature in the body of heater 1 is heated to about 1550 degrees centigrade, raw silicon 6 is all melted; Keeping body of heater 1 internal gas pressure is 600 millibars, closes well heater 8, and promotes heat-insulation cage 2 to 1/5th positions of crucible 7 height, makes the drop in temperature in the body of heater 1 and remains on about 1440 degrees centigrade, makes the silicon material 6 of fusing long brilliant; After 2 hours, keeping body of heater 1 internal gas pressure is 600 millibars, and with heat-insulation cage 2 minutes four times, contour 1/3rd positions that are promoted to crucible 7 height make temperature in the body of heater 1 from about 1440 degrees centigrade of left and right sides slow decreasings to 1410 degree centigrade; In the described step, keep this state 2 ~ 3 hours after promoting for the first time, keep this state about 7 hours after promoting for the second time, keep this state about 17 hours after promoting for the third time; Keep this state about 4 hours after last the lifting; In the meantime, the temperature in the body of heater 1 is from about 1440 degrees centigrade of left and right sides slow decreasings to 1410 degree centigrade, and body of heater 1 internal gas pressure is kept 600 millibars; In the above-mentioned steps, in long brilliant process, the solidification rate of silicon liquid is per hour carried out one-time detection; Keep body of heater 1 internal gas pressure and still be 600 millibars, about body of heater 1 interior drop in temperature to 1370 degree centigrade, heat-insulation cage 2 is dropped to graphite platform 3, and kept this state 3.5 hours, make the silicon ingot annealing behind the long crystalline substance; Increase the gas flow of air outlet 5, inlet mouth 4, keep body of heater 1 internal gas pressure and still be 600 millibars, approximately after 3 hours, heat-insulation cage is promoted to 2/3rds positions of crucible 7 height for 2 minutes three times, make about the drop in temperature to 400 degree centigrade in the body of heater 1; In the described step, heat-insulation cage 2 is promoted to 1/4th positions of crucible 7 height for the first time, body of heater 1 pressure increases to 700 millibars, and kept this state 2 hours, promote for the second time heat-insulation cage 2 to 1/2nd positions of crucible 7 height, and kept this state 7 ~ 8 hours, at last heat-insulation cage 2 is promoted to 2/3rds positions of crucible 7 height, close air outlet 5, air pressure in the body of heater 1 is forced into 850 millibars, keep this state about half an hour, make about the drop in temperature to 400 degree centigrade in the body of heater 1; Open at last body of heater 1, crucible 7 is taken out, and silicon ingot is naturally cooled to room temperature get final product.
In the implementation case, single stove polycrystal silicon ingot output from before 460 kilograms increase to 630 kilograms, the polycrystal silicon ingot utilization ratio of output from before 60 percent be increased to 70 percent, whole technique consuming time from before only increased to 70 hours in 63 hours; Further reduced cost, and out of use waste material still can advance the stove ingot casting again in the polycrystal silicon ingot after cleaning, and has improved utilization ratio.
Claims (8)
1. assorted material silicon is cast the polycrystal silicon ingot special furnace, comprise body of heater (1), described body of heater (1) is provided with inlet mouth (4) and air outlet (5), be provided with graphite platform (3) in the body of heater (1), be placed with crucible (7) on the described graphite platform (3), also comprise cover cap in the well heater (8) of crucible (7), cover cap is characterized in that in the heat-insulation cage (2) of well heater (8): the distance between described heat-insulation cage (2) inner top and graphite platform (3) upper surface is slightly less than 2 times of crucible (7) height.
2. a kind of assorted material silicon as claimed in claim 1 is cast the polycrystal silicon ingot special furnace, and it is characterized in that: the internal surface of described crucible (7) scribbles silicon nitride coating (9).
3. a kind of assorted material silicon as claimed in claim 2 is cast the polycrystal silicon ingot special furnace, and it is characterized in that: the internal surface in downward 3 ~ 8 cm range of crucible (7) limit mouth scribbles individual layer silicon nitride coating (9), and all the other internal surfaces scribble nitride multilayer silicon coating (9).
4. carry out the method for polycrystalline silicon ingot casting with above-mentioned assorted material silicon casting polycrystal silicon ingot special furnace, it is characterized in that may further comprise the steps:
The crucible (7) that 1) will fill raw silicon (6) is positioned over graphite platform (3), and with body of heater (1) closure;
2) heat-insulation cage (2) is promoted slightly, make between heat-insulation cage (2) bottom and graphite platform (3) upper surface gappedly, and pass through air outlet (5), with the interior vacuum pumping state of body of heater (1), body of heater (1) carries out preheating;
3) add protection gas by inlet mouth (4) in body of heater (1), the air pressure in the body of heater (1) is increased to 600 millibars gradually, heater (8) heats, and is heated to gradually about 1200 degrees centigrade in half an hour, and keeps about half an hour; Again the temperature in the body of heater (1) is heated to about 1550 degrees centigrade, with all fusings of raw silicon (6);
4) keeping body of heater (1) internal gas pressure is 600 millibars, close well heater (8), and promote heat-insulation cage (2) to 1/5th positions of crucible (7) height, and make the drop in temperature in the body of heater (1) and remain on about 1440 degrees centigrade, make the silicon material (6) of fusing long brilliant;
5) after 2 hours, keeping body of heater (1) internal gas pressure is 600 millibars, and heat-insulation cage (2) is divided four times, contour 1/3rd positions that are promoted to crucible (7) height, make temperature in the body of heater (1) from about 1440 degrees centigrade of left and right sides slow decreasings to 1410 degree centigrade;
6) keep body of heater (1) internal gas pressure and still be 600 millibars, about the drop in temperature to 1370 in the body of heater (1) degree centigrade, heat-insulation cage (2) is dropped to graphite platform (3), and kept this state 3.5 hours, make the silicon ingot annealing behind the long crystalline substance;
7) gas flow of increase air outlet (5), inlet mouth (4), keep body of heater (1) internal gas pressure and still be 600 millibars, approximately after 3 hours, heat-insulation cage (2) is promoted to 2/3rds positions of crucible (7) height minutes for three times, makes about the interior drop in temperature to 400 of body of heater (1) degree centigrade;
8) open body of heater (1), crucible (7) is taken out, and silicon ingot is naturally cooled to room temperature get final product.
5. a kind of assorted material silicon as claimed in claim 4 is cast the polycrystal silicon ingot method, it is characterized in that: in the described step 1), raw silicon comprises polysilicon and silicon single crystal in (6), the mass ratio of described polysilicon and silicon single crystal is 1:1, described silicon single crystal is as flavoring food, and the silicon single crystal flavoring food need to carry out annealing operation under the temperature about 550 degrees centigrade before ingot casting.
6. a kind of assorted material silicon casting polycrystal silicon ingot method as claimed in claim 4 is characterized in that: in the described step 5), in long brilliant process, the solidification rate of silicon liquid is per hour carried out one-time detection.
7. a kind of assorted material silicon as claimed in claim 4 is cast the polycrystal silicon ingot method, it is characterized in that: in the described step 5), keep this state 2 ~ 3 hours after promoting for the first time, keep this state about 7 hours after promoting for the second time, keep this state about 17 hours after promoting for the third time; Keep this state about 4 hours after last the lifting; In the meantime, the temperature in the body of heater (1) is from about 1440 degrees centigrade of left and right sides slow decreasings to 1410 degree centigrade, and body of heater (1) internal gas pressure is kept 600 millibars.
8. a kind of assorted material silicon as claimed in claim 4 is cast the polycrystal silicon ingot method, it is characterized in that: in the described step 7), heat-insulation cage (2) is promoted to 1/4th positions of crucible (7) height for the first time, body of heater (1) pressure increases to 700 millibars, and kept this state 2 hours, promote for the second time heat-insulation cage (2) to 1/2nd positions of crucible (7) height, and kept this state 7 ~ 8 hours, at last heat-insulation cage (2) is promoted to 2/3rds positions of crucible (7) height, close air outlet (5), air pressure in the body of heater (1) is forced into 850 millibars, keeps this state about half an hour.
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| CN201210426099.2A CN102925972B (en) | 2012-10-31 | 2012-10-31 | Special furnace for casting ingot from impurity silicon and ingot casting method using furnace |
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| CN201210426099.2A CN102925972B (en) | 2012-10-31 | 2012-10-31 | Special furnace for casting ingot from impurity silicon and ingot casting method using furnace |
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| CN102925972B CN102925972B (en) | 2015-07-22 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103436956A (en) * | 2013-08-12 | 2013-12-11 | 青岛隆盛晶硅科技有限公司 | Quick-melting and slow crystal growth high-efficiency polycrystalline silicon ingot casting process |
Citations (4)
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|---|---|---|---|---|
| EP0939146A1 (en) * | 1998-02-25 | 1999-09-01 | Mitsubishi Materials Corporation | Method for producing silicon ingot having directional solidification structure and apparatus for producing the same |
| CN102234837A (en) * | 2011-08-01 | 2011-11-09 | 浙江晶盛机电股份有限公司 | Closed cooling system of gas cooled polysilicon ingot furnace |
| CN102268728A (en) * | 2011-08-01 | 2011-12-07 | 上虞晶信机电科技有限公司 | Heat exchange platform of improved structure for polycrystalline silicon ingot furnace |
| CN102703976A (en) * | 2012-05-28 | 2012-10-03 | 北京工业大学 | Polycrystalline silicon furnace |
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2012
- 2012-10-31 CN CN201210426099.2A patent/CN102925972B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0939146A1 (en) * | 1998-02-25 | 1999-09-01 | Mitsubishi Materials Corporation | Method for producing silicon ingot having directional solidification structure and apparatus for producing the same |
| CN102234837A (en) * | 2011-08-01 | 2011-11-09 | 浙江晶盛机电股份有限公司 | Closed cooling system of gas cooled polysilicon ingot furnace |
| CN102268728A (en) * | 2011-08-01 | 2011-12-07 | 上虞晶信机电科技有限公司 | Heat exchange platform of improved structure for polycrystalline silicon ingot furnace |
| CN102703976A (en) * | 2012-05-28 | 2012-10-03 | 北京工业大学 | Polycrystalline silicon furnace |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103436956A (en) * | 2013-08-12 | 2013-12-11 | 青岛隆盛晶硅科技有限公司 | Quick-melting and slow crystal growth high-efficiency polycrystalline silicon ingot casting process |
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Effective date of registration: 20180413 Address after: 223700 No. 9 Guangdong Road, Siyang County Economic Development Zone, Jiangsu Patentee after: Jiangsu high & New Energy Technology Co., Ltd. Address before: 223700 Guangdong Road, economic development zone, Suqian, Jiangsu, No. 9 East Road, No. Patentee before: Suqian Yulong Photoelectric Technology Co., Ltd. |
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