CN101660200A - Method for growing polycrystalline silicon ingot under slight positive pressure state and ingot furnace - Google Patents
Method for growing polycrystalline silicon ingot under slight positive pressure state and ingot furnace Download PDFInfo
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- CN101660200A CN101660200A CN200910304181A CN200910304181A CN101660200A CN 101660200 A CN101660200 A CN 101660200A CN 200910304181 A CN200910304181 A CN 200910304181A CN 200910304181 A CN200910304181 A CN 200910304181A CN 101660200 A CN101660200 A CN 101660200A
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Abstract
The invention relates to a method for growing polycrystalline silicon ingot under slight positive pressure state and an ingot furnace. The method is to melt polycrystalline by adopting an air pressuremode of vacuumizing, and then filling argon till positive pressure state; and the ingot furnace is provided with an overpressure automatic relief valve and an anti-explosion valve. The polycrystalline silicon ingot grows under slight pressure, which can reduce dosage of argon, prevent gas from back flowing, ensure better safety, and can avoid oxidation of polycrystalline silicon ingot.
Description
Technical field
The present invention relates to a kind of method and apparatus of growing polycrystalline silicon ingot, be specifically related to the method and apparatus of growing polycrystalline silicon ingot under a kind of pressure-fired atmosphere.
Background technology
Polycrystalline silicon ingot or purifying furnace is in the photovoltaic industry, one of of paramount importance equipment.The polysilicon that is obtained by the polycrystalline silicon ingot casting method can directly obtain square material, and can make large-scale silicon ingot.
The principle of work of tradition polycrystalline silicon ingot or purifying furnace: be placed on the oriented solidified blocks after packing into polycrystalline silicon material in the cated crucible, vacuumize after closing burner hearth, after heating treats that the silicon material melts fully, heat-insulation cage slowly up promotes, the heat radiation that discharges during with the crystallization of silicon material by oriented solidified blocks makes and forms a vertical thermograde in the silicon material to the lower furnace chamber inwall.This thermograde makes the silicon liquid in the crucible begin to solidify from the bottom, from the melt bottom to grown on top.After the silicon material solidified, silicon ingot was annealed, come out of the stove after the cooling and promptly finish whole ingot casting process.
As mentioned above, present polycrystalline silicon ingot or purifying furnace all is to work under vacuum state, perhaps vacuumizes with applying argon gas and carries out simultaneously, and two kinds of working ordeies all are negative pressure state.Carry out polycrystalline silicon ingot casting under the negative pressure state, 2 weak points are arranged: 1, during the negative pressure melting, applying argon gas when vacuumizing keeps negative pressure, so the argon gas consumption is very big; Under the negative pressure state, if the equipment sealing is out of order suddenly, air can enter into suddenly in the burner hearth, and is very dangerous.
Summary of the invention
The objective of the invention is to overcome the deficiency that traditional polycrystalline silicon ingot or purifying furnace is worked under vacuum state, a kind of method and apparatus at growing polycrystalline silicon ingot under slight positive pressure state is provided.
Technical scheme one:
A kind of method of growing polycrystalline silicon ingot under slight positive pressure state may further comprise the steps:
Polycrystalline silicon material is packed in the quartz crucible, and the sealing furnace chamber is evacuated to 10-1Pa behind the open cycle water;
Begin to feed argon gas, the control argon flow amount after the furnace chamber stable gas pressure, is closed vacuum pump greater than vacuum pumping speed, and the air valve that begins to rehearse is adjusted argon flow amount, and making keep-ups pressure in the furnace chamber is 1.01～1.05 normal atmosphere;
Strengthen heating power gradually, carry out heat fused, crystallization, annealing, the cooling several steps, the furnace chamber internal pressure remains on 1.01～1.05 normal atmosphere in this process;
After step c finishes, close argon gas, take out polycrystalline silicon ingot casting.
The method of aforesaid a kind of growing polycrystalline silicon ingot under slight positive pressure state, wherein step a vacuum is: open sliding vane rotary pump earlier, change down and take out valve, when vacuum tightness reaches setting pressure, close and take out valve slowly, change up and take out valve, start lobe pump when vacuum tightness reaches setting pressure: reaching needs vacuum tightness.Close and take out the valve valve soon, detect the voltage rise rate, qualifiedly carry out next step operation.
Technical scheme two:
A kind of ingot furnace of growing polycrystalline silicon ingot under slight positive pressure state, comprise furnace chamber, be positioned at the outer well heater of the quartz crucible, quartz crucible of furnace chamber and connect the inflation system of furnace chamber, it is characterized in that: comprise that also a superpressure automatic blow off valve valve air relief and that is installed between venting port and the furnace chamber is installed in the furnace chamber wall the dual explosion trap between the inside and outside portion of furnace chamber.
The ingot furnace of aforesaid a kind of growing polycrystalline silicon ingot under slight positive pressure state, wherein said superpressure automatic blow off valve valve air relief comprises a pressure transmitter and rly. control electromagnetic release valve, pressure transmitter is set the feedback signal of furnace pressure, when reporting to the police during superpressure in the furnace chamber, by rly. control electromagnetic release valve automatic deflation, close automatically up to being lower than setting pressure.
The ingot furnace of aforesaid a kind of growing polycrystalline silicon ingot under slight positive pressure state, wherein said dual explosion trap comprises the flange that links to each other by pipeline with furnace chamber, valve outside flange and be located in flange and valve between aluminium foil, and be located at spring on the furnace wall, have the explosion trap air outlet on the described valve.
The ingot furnace of aforesaid a kind of growing polycrystalline silicon ingot under slight positive pressure state, when the furnace chamber internal pressure raises suddenly, spring has little time reaction, and when valve can't be opened, aluminium foil can be from the explosion trap air outlet by explosion, and gas is emitted from the explosion trap production well.
Produce the mode of polycrystalline silicon ingot casting compares with existing negative pressure of vacuum:
During the negative pressure melting, applying argon gas when vacuumizing keeps negative pressure, so the argon gas consumption is very big; Under the negative pressure state, if the equipment sealing is out of order suddenly, air can enter into suddenly in the burner hearth, and is very dangerous; During the pressure-fired melting, do not use vacuum pump, fill a small amount of argon gas and keep pressure-fired,,, reduce the work-ing life of vacuum pump simultaneously so can reduce very big kwh loss so the amount of applying argon gas seldom; Pressure-fired can prevent that gas from flowing backwards, and is safer, can prevent oxidation simultaneously.
Equipment of the present invention is provided with the superpressure automatic blow off valve valve air relief, when reporting to the police during superpressure in the furnace chamber, by rly. control electromagnetic release valve automatic deflation, closes automatically up to being lower than setting pressure; Dual explosion trap is installed on the furnace wall, has the explosion trap air outlet on the described dual explosion trap valve, when the furnace chamber internal pressure raises suddenly, spring has little time reaction, when valve can't be opened, aluminium is thin can be from the explosion trap air outlet by explosion, and gas is emitted from the explosion trap production well.By superpressure automatic blow off valve valve air relief and dual explosion trap, can protect the safety of ingot furnace well.
Description of drawings
Fig. 1 is the structural representation of the ingot furnace of a kind of growing polycrystalline silicon ingot under slight positive pressure state of the present invention, and wherein the A place is the explosion trap position;
Fig. 2 is the cross-sectional view of explosion trap;
Fig. 3 is the two dimensional structure synoptic diagram of explosion trap;
Fig. 4 is the structural representation of super automatic blow off valve valve air relief.
Embodiment
With reference to Fig. 1, the ingot furnace of a kind of growing polycrystalline silicon ingot under slight positive pressure state of the present invention comprises body of heater 1, establishes attemperator 5 in the body of heater 1, and well heater 6 is used to crucible 4 of placing polycrystalline silicon material etc.
Ingot furnace is connected with an inflation system, it comprise the last inflation valve that is installed on the gas ducting 7 and go up inflation glass rotameter 8 and following inflation valve 10 and under inflation glass rotameter 9.
One air-bleed system, it comprises takes out valve 13 slowly, takes out valve 15 and strainer 14 soon, a ZJP-300 lobe pump 12 and a sliding vane rotary pump 11.
In addition, ingot furnace of the present invention is provided with vent valve 17 and pressure regulator valve 16. at nearly venting port 19 places
For guaranteeing can to finish polycrystalline silicon ingot casting under positive pressure, must improve equipment, increase by a superpressure automatic blow off valve valve air relief and an explosion trap:
(1), a superpressure automatic blow off valve valve air relief 3 is set between furnace chamber 1 and venting port 19.
With reference to Fig. 1 and Fig. 4, superpressure automatic blow off valve valve air relief 3 is made up of pressure transmitter 31 and rly. control electromagnetic release valve 32 simultaneously.Pressure transmitter 31 is set the feedback signal of furnace pressures, when reporting to the police during superpressure in the furnace chamber, by rly. control electromagnetic release valve 32 automatic deflations, closes automatically up to being lower than setting pressure.
(2), on the wall of furnace chamber 1, establish an explosion trap 2
With reference to figure 2 and Fig. 3, explosion trap 2 is a dual explosion trap, can suit simultaneously to work under malleation and the negative pressure simultaneously, and it mainly comprises spring 21, and spring 21 is installed on the furnace wall 22; Flange 25 links to each other by pipeline 27 with furnace chamber; Aluminium foil 24 is located between flange 25 and the valve 27.Some production wells 26 are arranged on the valve 27, between valve 27 and the flange 25 sealing-ring 23 is arranged.When the pressure in the furnace chamber surpassed the pressure of spring 21 settings, valve 27 was opened automatically; When the furnace chamber internal pressure was lower than spring 21 setting pressures, under the reactive force of spring 21, valve 27 was withdrawn automatically.When the furnace chamber internal pressure raises suddenly, spring 21 has little time reaction, and when valve 27 can't be opened, aluminium foil can be from production well 26 explosions, pressure release, and gas is emitted from explosion trap production well 26.
During use,
Polycrystalline silicon material is packed in the quartz crucible, and the sealing furnace chamber vacuumizes behind the open cycle water;
Open inflation valve, be inflated to setting pressure, inflation valve is closed automatically, continues to vacuumize to reach vacuum tightness, inflates again; Guarantee vacuum tightness according to processing requirement, vacuum is evacuated to 10
-1Pa gets final product;
Begin to feed argon gas, the control argon flow amount after the furnace chamber stable gas pressure, is closed vacuum pump greater than vacuum pumping speed, and the air valve that begins to rehearse is adjusted argon flow amount, and making keep-ups pressure in the furnace chamber is 1.01～1.05 normal atmosphere;
Strengthen heating power gradually, carry out heat fused, crystallization, annealing, the cooling several steps, the furnace chamber internal pressure keeps 1.01～1.05 in this process;
After steps d is finished, close argon gas, take out polycrystalline silicon ingot casting.
Ingot furnace is worked under pressure-fired, reduce, reduced the cost of manufacture of ingot furnace simultaneously for the ingot furnace vacuum requirements.Melting polysilicon under the pressure-fired has mainly reduced the oxygen level in the silicon ingot, has also reduced the impurity on ingot casting surface.
Above-mentioned only is a specific embodiment of the present invention, but design concept of the present invention is not limited thereto, and allly utilizes this design that the present invention is carried out the change of unsubstantiality, all should belong to the behavior of invading protection domain of the present invention.
Claims (5)
1. the method for a growing polycrystalline silicon ingot under slight positive pressure state may further comprise the steps:
A, polycrystalline silicon material is packed in the quartz crucible, the sealing furnace chamber vacuumizes behind the open cycle water;
B, feeding argon gas, the control argon flow amount after the furnace chamber stable gas pressure, is closed vacuum pump greater than vacuum pumping speed, and the air valve that begins to rehearse is adjusted argon flow amount, and making keep-ups pressure in the furnace chamber is 1.01～1.05 normal atmosphere;
C, strengthen heating power gradually, carry out the heat fused of polysilicon, crystallization, annealing, the cooling several steps, the furnace chamber internal pressure keeps 1.01～1.05 normal atmosphere in this process;
After d, step c finish, close argon gas, take out polycrystalline silicon ingot casting.
2. the ingot furnace of a growing polycrystalline silicon ingot under slight positive pressure state, comprise furnace chamber, be positioned at the outer well heater of the quartz crucible, quartz crucible of furnace chamber and connect the inflation system of furnace chamber, it is characterized in that: comprise that also a superpressure automatic blow off valve valve air relief and that is installed between venting port and the furnace chamber is installed in the furnace chamber wall the dual explosion trap between the inside and outside portion of furnace chamber.
3. the ingot furnace of a kind of growing polycrystalline silicon ingot under slight positive pressure state as claimed in claim 2, it is characterized in that: described superpressure automatic blow off valve valve air relief comprises a pressure transmitter and rly. control electromagnetic release valve, described pressure transmitter can be set the feedback signal of furnace pressure, when reporting to the police during superpressure in the furnace chamber, by rly. control electromagnetic release valve automatic deflation, close automatically up to being lower than setting pressure.
4. the ingot furnace of a kind of growing polycrystalline silicon ingot under slight positive pressure state as claimed in claim 2, it is characterized in that: described dual explosion trap comprises the flange that links to each other by pipeline with furnace chamber, valve outside flange and be located in flange and valve between aluminium foil, and be located at spring on the furnace wall, have the explosion trap air outlet on the described valve.
5. the ingot furnace of a kind of growing polycrystalline silicon ingot under slight positive pressure state as claimed in claim 4, it is characterized in that: when the furnace chamber internal pressure raises suddenly, spring has little time reaction, when valve can't be opened, aluminium foil can be from the explosion trap air outlet by explosion, and gas is emitted from the explosion trap production well.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009103041816A CN101660200B (en) | 2009-07-09 | 2009-07-09 | Method for growing polycrystalline silicon ingot under slight positive pressure state and ingot furnace |
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| CN2009103041816A CN101660200B (en) | 2009-07-09 | 2009-07-09 | Method for growing polycrystalline silicon ingot under slight positive pressure state and ingot furnace |
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| CN101660200B CN101660200B (en) | 2011-12-28 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102978709A (en) * | 2012-11-16 | 2013-03-20 | 晶科能源有限公司 | Efficient cooling technical method of polycrystal ingot casting |
| CN108707962A (en) * | 2018-06-29 | 2018-10-26 | 天津市环欧半导体材料技术有限公司 | A kind of protective device for adjusting zone melting furnace pressure |
| CN113584586A (en) * | 2021-08-06 | 2021-11-02 | 宁夏红日东升新能源材料有限公司 | Method and device for purifying polycrystalline silicon by centrifugal directional solidification |
-
2009
- 2009-07-09 CN CN2009103041816A patent/CN101660200B/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102978709A (en) * | 2012-11-16 | 2013-03-20 | 晶科能源有限公司 | Efficient cooling technical method of polycrystal ingot casting |
| CN102978709B (en) * | 2012-11-16 | 2016-04-06 | 晶科能源有限公司 | A kind of technological method of polycrystalline cast ingot high efficiency cooling |
| CN108707962A (en) * | 2018-06-29 | 2018-10-26 | 天津市环欧半导体材料技术有限公司 | A kind of protective device for adjusting zone melting furnace pressure |
| CN113584586A (en) * | 2021-08-06 | 2021-11-02 | 宁夏红日东升新能源材料有限公司 | Method and device for purifying polycrystalline silicon by centrifugal directional solidification |
| CN113584586B (en) * | 2021-08-06 | 2024-04-26 | 宁夏红日东升新能源材料有限公司 | Centrifugal directional solidification purification method and device for polysilicon |
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