CN106048718B - A kind of polysilicon fritting ingot casting sundries discharging method - Google Patents
A kind of polysilicon fritting ingot casting sundries discharging method Download PDFInfo
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- CN106048718B CN106048718B CN201610696080.8A CN201610696080A CN106048718B CN 106048718 B CN106048718 B CN 106048718B CN 201610696080 A CN201610696080 A CN 201610696080A CN 106048718 B CN106048718 B CN 106048718B
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/04—Production of homogeneous polycrystalline material with defined structure from liquids
- C30B28/06—Production of homogeneous polycrystalline material with defined structure from liquids by normal freezing or freezing under temperature gradient
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
Abstract
The invention discloses a kind of polysilicon fritting ingot casting sundries discharging methods, including step：One, fusing and impurities removal, process are as follows：101, it melts：Using polycrystalline silicon ingot or purifying furnace to being melted loaded on the silicon material in crucible, and it is filled with inert gas into polycrystalline silicon ingot or purifying furnace and carries out pressurize；102, it is depressured impurities removal；103, later stage impurities removal is melted：First the air pressure of polycrystalline silicon ingot or purifying furnace is boosted, then silicon material is continued to melt, and makes 0.8≤c ＜ 1, c be that coefficient is compared in the top side of polycrystalline silicon ingot or purifying furnace by adjusting the heating power of top heater and/or four side heaters；Two, long crystalline substance and synchronous impurities removal：Make 0.3≤c ＜ 0.9 by adjusting the heating power of top heater and/or four side heaters.The method of the present invention step is simple, reasonable design and realization are easy, using effect, and the Hard Inclusion of ingot casting finished product is effectively reduced by the synchronization impurities removal of melt later stage, decompression impurities removal impurities removal synchronous with long crystalline substance process, can effectively improve the quality of ingot casting finished product.
Description
Technical field
The invention belongs to polycrystalline silicon ingot casting technical fields, more particularly, to a kind of polysilicon fritting ingot casting sundries discharging method.
Background technology
Photovoltaic generation is one of currently the most important clean energy resource, has great development potentiality.Restrict photovoltaic industry hair
On the one hand the key factor of exhibition is that electricity conversion is low, is on the other hand high expensive.Photovoltaic silicon wafer is production solar-electricity
The basic material in pond and component, for produce photovoltaic silicon wafer polysilicon purity must (i.e. non-silicon impurities always contain at 6N grades or more
Amount is in 1ppm or less), otherwise the performance of photovoltaic cell will be by prodigious negative effect.In recent years, polysilicon chip production technology
There are marked improvement, polycrystalline cast ingot technology to be arrived from G4 (each silicon ingot weighs about 270 kilograms, can cut 4 × 4=16 silicon side) progress
G5 (5 × 5=25 silicon side), then G6 (6 × 6=36 silicon side) is arrived in progress again.Also, the unit of produced polycrystalline silicon ingot casting
Volume incrementally increases, and yield rate increases, and the manufacturing cost of unit volume polycrystalline silicon ingot casting gradually reduces.Actual production process
In, when solar energy polycrystalline silicon ingot casting, silicon material need to be loaded using silica crucible, and after silicon material is put into silica crucible, usual feelings
Preheated, fusing (also referred to as melt) is also needed under condition, long brilliant (also referred to as directional solidification crystallization), anneals, cool down, and could be completed
Polycrystalline silicon ingot casting process.Currently, in photovoltaic industry technology industry, the improvement of polycrystal silicon ingot foundry engieering is to reduce battery cost
One of main path.The impurity such as Hard Inclusion can be all formed comprising impurity and oxygen and influence turning for solar cell in casting polysilicon
Change efficiency.
Currently, polycrystalline silicon ingot casting method mainly has two kinds of half casting process and fine melt ingot casting method.Wherein, half casting process
(also referred to as have seed crystal ingot casting polycrystalline silicon process, have seed crystal high-efficiency polycrystalline silicon technology, fritting height to follow) refers to using grade silicon
Material carries out epitaxial growth as nucleating center, casts the polycrystalline silicon ingot casting of low defect high-quality；Fine melt ingot casting method is (also referred to as without seed
Brilliant ingot casting polycrystalline silicon process is followed without seed crystal high-efficiency polycrystalline silicon technology, fine melt height), refer to using non-silicon material in crucible bottom
Prepare shaggy heterogeneous forming core layer, degree of supercooling obtains larger forming core when roughness and forming core by controlling forming core layer
Rate casts low defect high-quality polycrystalline silicon ingot casting.Seed crystal high-efficiency polycrystalline silicon technology is the epitaxial growth of silicon materials, and without seed crystal
High-efficiency polycrystalline silicon technology is a kind of heterogeneous forming core；Although the little crystal grain efficient polycrystalline silicon ingot casting of high-quality both can be obtained,
But due to nucleating mechanism difference, the crystalline silicon of two kinds of technology growths has a certain difference.
During carrying out polycrystalline silicon ingot casting using half casting process, crucible bottom is layered on as seed using polycrystalline silicon fragments
Crystalline substance controls the burn-off rate of silicon material in fusion process, ensures the silicon of bottom residue 1cm~2cm thickness in the end of melting step
Material, remaining silicon material is as long brilliant required seeding material.The experimental results showed that：Half casting process can reduce silicon ingot bottom crystalline substance
Flower size reduces silicon ingot internal crystal framework dislocation ratio, and the brilliant process of silicon ingot length can keep vertical substantially during fritting ingot casting
Direction is grown, and test result shows that the silicon ingot transfer efficiency of half casting process turns than the silicon ingot of the fine melt ingot casting method under equal conditions
It changes efficient.Currently, the advantages that fritting casting ingot process of solar energy polycrystalline silicon ingot casting has been spent with its crystalline substance is pushed away by the consistent of market
Extensively, however since the silicon material of crucible side has not melted in fritting casting ingot process, the impurity and oxygen in raw material do not obtain effectively
Impurities removal, cause these impurity to form Hard Inclusion during ingot casting, have a great impact to the quality of product.Existing fritting
Casting ingot process can be accomplished to control the Hard Inclusion of ingot casting finished product in 3%~5% percentage point, and fluctuation range is larger, and this number
According to the data for being cant flaw detection, quasi- number formulary is according to higher and Hard Inclusion ratio up to 5% or more.
Invention content
In view of the above-mentioned deficiencies in the prior art, the technical problem to be solved by the present invention is that providing a kind of polysilicon half
Founding ingot sundries discharging method, method and step is simple, reasonable design and realization are easy, using effect, is synchronized by the melt later stage
Impurities removal, decompression impurities removal impurities removal synchronous with long crystalline substance process effectively reduce the Hard Inclusion of ingot casting finished product, can effectively improve ingot casting finished product
Quality.
In order to solve the above technical problems, the technical solution adopted by the present invention is：A kind of polysilicon fritting ingot casting impurities removal side
Method, which is characterized in that this approach includes the following steps：
Step 1: fusing and impurities removal, process are as follows：
Step 101, fusing：By in polycrystalline silicon ingot or purifying furnace be located at crucible above top heater and four be laid in respectively
After the side heater of four side-wall outer sides of crucible is opened, according to conventional half casting process of polysilicon, using polysilicon
For ingot furnace to being melted loaded on the silicon material in crucible, fusion temperature is T1~T2；Wherein, T1=1125 DEG C~1285 DEG C, T2
=1530 DEG C~1550 DEG C；
It is carried out in fusion process in step 101, inert gas is filled with into polycrystalline silicon ingot or purifying furnace and by polycrystalline silicon ingot or purifying furnace
Interior air pressure is maintained at Q1, wherein Q1=550mbar~650mbar；
Step 102, decompression impurities removal, process are as follows：
Step 1021, decompression：By the heating and temperature control of polycrystalline silicon ingot or purifying furnace in T2, and by the air pressure of polycrystalline silicon ingot or purifying furnace
Q2 is down to by Q1, dip time is 8min~12min；Wherein, Q2=350mbar~450mbar；
Step 1022, pressurize：By the heating and temperature control of polycrystalline silicon ingot or purifying furnace in T2, and by air pressure in polycrystalline silicon ingot or purifying furnace
It is maintained at Q2, the dwell time is 10min~60min；
Step 103, fusing later stage impurities removal：The air pressure of polycrystalline silicon ingot or purifying furnace is first risen into Q1 by Q2, then is cast using polysilicon
For ingot stove to continuing to melt loaded on the silicon material in crucible, continuation fusing time is 15min~40min；
Continue in fusion process, by adjusting top heater and/or the heating power of four side heaters, makes
0.8≤c ＜ 1, and the heating temperature of polycrystalline silicon ingot or purifying furnace is made gradually to be down to T3 from T2；Wherein, T3 be polysilicon crystal temperature and
T3=1420 DEG C~1440 DEG C；
Wherein, c be the top side of polycrystalline silicon ingot or purifying furnace than coefficient andcdingFor the power ratio system of top heater
Number andPdFor the practical heating power of top heater, PdmaxFor the maximum heating power of top heater；PcFor the practical heating power of side heater, PcmaxFor the maximum heating power of side heater；Pdmax＜
Pcmax；
Step 2: long brilliant and synchronous impurities removal：In step 1 fusing and impurities removal after the completion of, proceed by directional solidification and enter
Long crystalline substance process；During long crystalline substance, by adjusting top heater and/or the heating power of four side heaters, make 0.3
≤ c ＜ 0.9.
A kind of above-mentioned polysilicon fritting ingot casting sundries discharging method, it is characterized in that：Top heater described in step 1 passes through
First electrode is connect with top heating power supply, and four side heaters are connected by second electrode and side heating power supply
It connects；The top heating power supply and side heating power supply are connect with heating power regulating device, and the heating power adjusts dress
It is set to the PCU Power Conditioning Unit that the output power of top heating power supply and side heating power supply is adjusted respectively.
A kind of above-mentioned polysilicon fritting ingot casting sundries discharging method, it is characterized in that：Four sides in step 1 and step 2
The heating power all same of portion's heater；.
A kind of above-mentioned polysilicon fritting ingot casting sundries discharging method, it is characterized in that：Top described in step 1 and step 2 adds
The practical heating power of hot device is 70kW~90kW；P described in step 1dmax150kW~180kW, Pcmax=220kW~
260kW。
A kind of above-mentioned polysilicon fritting ingot casting sundries discharging method, it is characterized in that：When being melted in step 101, including with
Lower step：
Step 1011, heating：The heating temperature of polycrystalline silicon ingot or purifying furnace is stepped up from T1 to T2；In temperature-rise period, institute
It states air pressure in polycrystalline silicon ingot or purifying furnace and is maintained at Q1；Wherein Q1=550mbar~650mbar；
In this step, the top side of the polycrystalline silicon ingot or purifying furnace is than coefficient c=1；
Step 1012 is kept the temperature for the first time：By the heating and temperature control of polycrystalline silicon ingot or purifying furnace in T2, and keep the temperature 4h~8h；It protects
During temperature, in the polycrystalline silicon ingot or purifying furnace air pressure be maintained at Q1；
In this step, the top side of the polycrystalline silicon ingot or purifying furnace is than coefficient c=1；
Step 1013 is kept the temperature for second：By the heating and temperature control of polycrystalline silicon ingot or purifying furnace in T2, and keep the temperature 10h~14h；
In insulating process, in the polycrystalline silicon ingot or purifying furnace air pressure be maintained at Q1；
In this step, by adjusting top heater and/or the heating power of four side heaters, make 0.9≤c
＜ 1.3.
A kind of above-mentioned polysilicon fritting ingot casting sundries discharging method, it is characterized in that：It was kept the temperature for the second time in step 1013
Cheng Zhong makes c be gradually decrease to from 1.2 by adjusting top heater and/or the heating power of four side heaters
0.95。
A kind of above-mentioned polysilicon fritting ingot casting sundries discharging method, it is characterized in that：Later stage impurities removal process is melted in step 103
In, by adjusting top heater and/or the heating power of four side heaters, c is made to be gradually decrease to from 0.95
0.8。
A kind of above-mentioned polysilicon fritting ingot casting sundries discharging method, it is characterized in that：Long brilliant and synchronous impurities removal is carried out in step 2
Before, the heating temperature of polycrystalline silicon ingot or purifying furnace is first down to T4 from T3, wherein T4=1410 DEG C~1430 DEG C；
When carrying out long brilliant and synchronous impurities removal in step 2, include the following steps：
Step 201, length crystalline substance early period and synchronous removal of impurities：The heating temperature of polycrystalline silicon ingot or purifying furnace is gradually risen into T3 from T4, and
By adjusting top heater and/or the heating power of four side heaters, make c from c1It is gradually decrease to c0；Wherein c1
=0.8~0.9, c0=0.3~0.6；The early period length brilliant time is 10h~15h；
Step 202, later stage length are brilliant and synchronize removal of impurities：The heating temperature of polycrystalline silicon ingot or purifying furnace is gradually down to T5 from T3, and
By adjusting top heater and/or the heating power of four side heaters, make c from c0Gradually increase to 1；Wherein T5=
1405 DEG C~1425 DEG C；The later stage length brilliant time is 28h~35h.
A kind of above-mentioned polysilicon fritting ingot casting sundries discharging method, it is characterized in that：Long brilliant and synchronous impurities removal is carried out in step 2
In the process, long brilliant rate control is in 10mm/h~13mm/h.
A kind of above-mentioned polysilicon fritting ingot casting sundries discharging method, it is characterized in that：When being melted in step 101, crucible is waited for
When the thickness of inside bottom silicon material is 13mm~20mm, fusing is completed.
Compared with the prior art, the present invention has the following advantages：
1, reasonable design and treatment process steps are simple, is easy to grasp.
2, input cost is low and realizes conveniently.
3, easy to use, the fusing later stage and it is long brilliant during by adjusting top heater and side heater plus
Thermal power achievees the purpose that effective impurities removal.Also, it controls easy and realizes conveniently, pass through tune during phase and length are brilliant after being melted down
The heating power of whole top heater and side heater controls the top side ratio coefficient of polycrystalline silicon ingot or purifying furnace, while in long brilliant process
The long brilliant rate of middle control.
4, long brilliant Process Design is reasonable, long brilliant in the process by controlling long brilliant rate and top side ratio coefficient, reaches length of side crystalline substance
The purpose of side impurities removal can effectively reduce the Hard Inclusion in cast ingot product, and can drop to the Hard Inclusion data stabilization that quasi- side detects a flaw
Within 1%.
5, fusion process is easy and is easy to grasp, and first the heating temperature of polycrystalline silicon ingot or purifying furnace is stepped up to polysilicon
Fusion temperature, then the constant progress first time heat preservation of heating temperature and the heat preservation 4h~8h of polycrystalline silicon ingot or purifying furnace are controlled, it controls later
The constant progress of heating temperature of polycrystalline silicon ingot or purifying furnace is kept the temperature for the second time and heat preservation 10h~14h；It is first fast subsequently into decompression impurities removal
Speed reduces air pressure in stove, and quickly reducing air pressure helps that foreign gas is quickly discharged, and inhibition carbonaceous gas and melted silicon connect
It touches and adsorbs；Contribute to the fusing of further promotion silicon liquid simultaneously；It reduces rapidly in stove after air pressure, then pressurize 10~60min mistakes
So that carbon-containing impurities enhance the convection current of melt and bath surface, it is made fully to arrange no longer in stove body-internal-circulation in gas in journey
Miscellaneous, furnace body is discharged with air-flow in impurity, thus can effectively reduce impurity inside furnace chamber using decompression impurities removal, is easy in crystal growing stage
Higher clean crystals growing environment is obtained, the carbon content in silicon ingot growth course (i.e. crystal growing stage) can be effectively reduced, to
So that the silicon ingot of growth is had higher quality, and the generation of Hard Inclusion can be effectively reduced to improve silicon ingot yield rate, and reduces silicon
Piece cuts breakage ratio, improves solar battery sheet yield rate and transfer efficiency；It is depressured after the completion of impurities removal, into fusing later stage impurities removal
Process specifically uses polycrystalline silicon ingot or purifying furnace to carrying out continuing to melt loaded on the silicon material in crucible, and continuation fusing time is 15min
~40min.After the completion of melting later stage impurities removal process, fusion process terminates.Fusion process reasonable design is realized convenient and uses effect
Fruit is good, can be effectively improved crystal growth quality, reduces and glues crucible rate, improves the transfer efficiency of solar battery sheet, can effectively improve finished product
Rate.Meanwhile it can be accurately melted to the switching time of crystal growing stage, prevent since the melt time is insufficient or melt overlong time is made
At polycrystalline silicon ingot casting quality decline, cost increase the problems such as.Also, using the present invention to melt during polycrystalline silicon ingot casting extremely
After long brilliant switching time is accurately held, it can ensure that the quality of long crystalline substance and be finally made the transfer efficiency of cell piece.Meanwhile
It is smooth to melt later stage liquid level.
6, sundries discharging method is simple, reasonable design and impurities removal effect are good, including impurities removal process three times, respectively melt later stage are same
Walk impurities removal, decompression impurities removal impurities removal synchronous with long crystalline substance process；Wherein, the fusing later stage is by adjusting top heater and side heater
Heating power control top side synchronize impurities removal than coefficient, it is miscellaneous that decompression impurities removal by decompression and pressurize effectively reduces furnace chamber inside
Matter simultaneously accordingly reduces the carbon content in silicon ingot growth course and realizes impurities removal, at the same during long brilliant by control long brilliant rate and
It realizes length of side crystal edge impurities removal than coefficient, plays the role of impurities removal three times in top side.It is used with existing polysilicon fritting casting ingot process
Long crystal type is compared after first impurities removal, and the present invention need not change the heater structure in polycrystalline silicon ingot or purifying furnace, easy to operate, is only needed
Change technological parameter is the purpose that can reach effective impurities removal and improve product quality, can be by Hard Inclusion data stabilization that quasi- side detects a flaw
It drops within 1%.Thus, impurities removal technique of the present invention can effectively reduce the impurity content in silicon material, to make life
Long silicon ingot has higher quality, and can effectively reduce the generation of Hard Inclusion to improve silicon ingot yield rate, and reduces silicon chip and cut
Breakage ratio is cut, the yield rate of silicon ingot is improved and the overall conversion efficiency of solar battery sheet, the sundries discharging method is easy to operate, practical
Property it is strong, convenient for batch production.
7, polycrystalline silicon ingot or purifying furnace internal heater is individually controlled using dual power supply, need not be changed in polycrystalline silicon ingot or purifying furnace
Heater structure, input cost is low and realizes convenient, and top heater and side heater use separate power supply, top
Portion's heater and side heater can be controlled individually and the heating power of the two can be separated and individually be controlled, and be controlled at this time
Mode has the following advantages：The first, more energy saving, it is not necessary to which that top heater and side heater are using same heating work(
Rate to achieve the purpose that reduce h eating power, while can effectively reduce the heat that cooling water is taken away in the unit interval, between
Ground connection reduces the load of power refrigeration equipment；The second, thermal field can be preferably controlled, due to top heater and side heater
It can individually be controlled, the purpose that easy can be realized top heater and side heater and separately heat is effective so as to reach
Control the purpose of thermal field；Third has prodigious improvement result for crystal growing process, is conducive in polycrystalline silicon ingot or purifying furnace
Portion forms vertical gradient thermal field evenly, to preferably control long brilliant rate so that long crystal boundary face is gentler, to subtract
The unfavorable factors such as few shade, red sector, heating effect is more preferably；4th, it can effectively mitigate the load carried on main line, effectively reduce
Electric current superposition amount on main line has busbar and switchgear house certain protective effect to reduce line load amount；The
Five, the service life of internal thermal field can be extended.
8, long brilliant process control is simple, realizes that convenient and using effect is good, not only simplifies polycrystalline silicon ingot casting crystal growing technology
Step, temperature, which controls, during keeping entire length brilliant more they tends to stable state, can achieve the purpose of energy saving, while in long crystalline substance mistake
Cheng Zhongneng, which is synchronized, carries out impurities removal, can effectively improve crystal growth quality, reduces Hard Inclusion, reduce and glue crucible rate, improves solar battery sheet
Transfer efficiency, this method is easy to operate, highly practical, convenient for batch production.Meanwhile long brilliant speed is carried out during long crystalline substance
Rationally control, and after the long brilliant process of rationally control, can ensure that the quality of long crystalline substance and the transfer efficiency of cell piece is made.Thus, this
Crystal growing technology more stabilizes silicon ingot growth course used by invention, provides preferable environment for long brilliant process, avoids growing
Microdefect caused by during brilliant, enhances practicability, convenient for batch production.
9, highly practical, convenient for batch production.
In conclusion the method for the present invention step is simple, reasonable design and realization are easy, using effect, pass through the melt later stage
Synchronous impurities removal, decompression impurities removal impurities removal synchronous with long brilliant process effectively reduce the Hard Inclusion of ingot casting finished product, can effectively improve ingot casting at
The quality of product.
Below by drawings and examples, technical scheme of the present invention will be described in further detail.
Description of the drawings
Fig. 1 is the method flow block diagram of the present invention.
Fig. 2 is the layout position illustration of polycrystalline silicon ingot or purifying furnace inner top heater and side heater of the present invention.
Fig. 3 is top heater of the present invention, the schematic block circuit diagram of side heater and heating power regulating device.
Reference sign:
1-crucible；2-top heaters；2-1-top heating power supply；
3-polycrystalline silicon ingot or purifying furnaces；4-side heaters；4-1-side heating power supply；
5-DS blocks；6-heating power regulating devices；7-crucible guard boards；
8-heat-preservation cylinders；9-pressure pins.
Specific implementation mode
Embodiment 1
A kind of polysilicon fritting ingot casting sundries discharging method as shown in Figure 1, includes the following steps：
Step 1: fusing and impurities removal, process are as follows：
Step 101, fusing：By the top heater 2 and four difference cloth in polycrystalline silicon ingot or purifying furnace 3 above crucible 1
Be located at four side-wall outer sides of crucible 1 side heater 4 open after, according to conventional half casting process of polysilicon, use
For polycrystalline silicon ingot or purifying furnace 3 to being melted loaded on the silicon material in crucible 1, fusion temperature is T1~T2；Wherein, T1=1200 DEG C, T2
=1540 DEG C；
It is carried out in fusion process in step 101, inert gas is filled with into polycrystalline silicon ingot or purifying furnace 3 and by polycrystalline silicon ingot or purifying furnace
Air pressure is maintained at Q1, wherein Q1=600mbar in 3；
Step 102, decompression impurities removal, process are as follows：
Step 1021, decompression：By the heating and temperature control of polycrystalline silicon ingot or purifying furnace 3 in T2, and by the gas of polycrystalline silicon ingot or purifying furnace 3
Pressure is down to Q2, dip time 10min by Q1；Wherein, Q2=400mbar；
Step 1022, pressurize：By the heating and temperature control of polycrystalline silicon ingot or purifying furnace 3 in T2, and by gas in polycrystalline silicon ingot or purifying furnace 3
Pressure is maintained at Q2, dwell time 30min；
Step 103, fusing later stage impurities removal：The air pressure of polycrystalline silicon ingot or purifying furnace 3 is first risen into Q1 by Q2, then is cast using polysilicon
For ingot stove 3 to continuing to melt loaded on the silicon material in crucible 1, continuation fusing time is 35min；
Continue in fusion process, by adjusting top heater 2 and/or the heating power of four side heaters 4,
Make 0.8≤c ＜ 1, and the heating temperature of polycrystalline silicon ingot or purifying furnace 3 is made gradually to be down to T3 from T2；Wherein, T3 is polysilicon crystal temperature
And T3=1430 DEG C；
Wherein, c be the top side of polycrystalline silicon ingot or purifying furnace 3 than coefficient andcdingFor the power ratio of top heater 2
Coefficient andPdFor the practical heating power of top heater 2, PdmaxFor the maximum heating work(of top heater 2
Rate；PcFor the practical heating power of side heater 4, PcmaxFor the maximum heating power of side heater 4；
Pdmax＜ Pcmax；
Step 2: long brilliant and synchronous impurities removal：In step 1 fusing and impurities removal after the completion of, proceed by directional solidification and enter
Long crystalline substance process；During long crystalline substance, by adjusting top heater 2 and/or the heating power of four side heaters 4, make
0.3≤c ＜ 0.9.
In actual use, when the air pressure of polycrystalline silicon ingot or purifying furnace 3 being risen to Q1 by Q2 in step 103, pressure rising time 8min
~12min.
In actual use, the size of T1, T2 and T3 can be adjusted accordingly according to specific needs.Wherein, T2 is
Unmelted polycrystalline silicon temperature.Also, it can according to specific needs, to continuing to melt in the fusing time and step 102 in step 101
Time adjusts accordingly respectively.
Currently, polycrystalline silicon ingot casting method mainly has two kinds of half casting process and fine melt ingot casting method, half casting process is also referred to as
There is seed crystal ingot casting polycrystalline silicon process, refers to that epitaxial growth, casting low defect Gao Pin are carried out as nucleating center using grade silicon material
The polycrystalline silicon ingot casting of matter；Fine melt ingot casting method is also referred to as
Shaggy heterogeneous forming core layer is prepared in crucible bottom using non-silicon material, by control forming core layer roughness and forming core when
Degree of supercooling obtains larger nucleation rate, casts low defect high-quality polycrystalline silicon ingot casting.In the present embodiment, melted in step 1
Before, it first feeds according to the loading method of conventional half casting process.As shown in Fig. 2, after the completion of charging, crucible 1 is placed
In on the DS blocks 5 in polycrystalline silicon ingot or purifying furnace 3.Wherein, DS blocks 5 are graphite block, and the thermal conductivity of the graphite block is very strong.The DS blocks
5 are also referred to as directional solidification block or DS-BLOCK.Heat-preservation cylinder 8 is provided in the polycrystalline silicon ingot or purifying furnace 3.And then according to routine
The pre-heating mean of half casting process preheats the silicon material in crucible 1.After the completion of preheating, then proceed by fusing.
In the present embodiment, the polycrystalline silicon ingot or purifying furnace 3 is G5 type ingot furnaces.Also, the polycrystalline silicon ingot or purifying furnace 3 is specially
The G5 type ingot furnaces of Zhejiang Jingsheng Electrical and Mechanical Co., Ltd.'s production.The crucible 1 be silica crucible and its be G5 crucibles, and
The polycrystalline silicon ingot casting produced is G5 ingots.
In actual use, the charge of the silica crucible is 600kg or so.
In the present embodiment, the charge of the silica crucible is 560kg.It in actual use, can be according to specific need
It wants, the charge of the silica crucible is adjusted accordingly.
In the present embodiment, as shown in Figure 2 and Figure 3, top heater 2 described in step 1 is added by first electrode and top
Thermoelectric generator 2-1 connections, four side heaters 4 are connect by second electrode with side heating power supply 4-1；The top
Heating power supply 2-1 and side heating power supply 4-1 are connect with heating power regulating device 6, and the heating power regulating device 6 is
The PCU Power Conditioning Unit that the output power of top heating power supply 2-1 and side heating power supply 4-1 are adjusted respectively.
The top heating power supply 2-1 and side heating power supply 4-1 is power adjustable economize on electricity source, and top heater
2 and four side heaters 4 two different power supplys (the i.e. described top heating power supply and side heating is respectively adopted
Power supply), it can realize that the independent control of top heater 2 and side heater 4, easy to use and using effect are good.
In the present embodiment, the heating power regulating device 6 includes two heating power adjustment equipments, is added described in two
Thermal power adjustment equipment is respectively the first heating power adjustment equipment that the heating power of top heater 2 is adjusted and right
The second heating power adjustment equipment that the heating power of four side heaters 4 is adjusted synchronously.
In actual use, two heating power adjustment equipments can also share a heating power adjusting and set
It is standby, it only needs to achieve the purpose that be respectively controlled two power supplys.
In the present embodiment, the top heater 2 and side heater 4 are the existing of existing polycrystalline silicon ingot or purifying furnace use
The structure and installation position of heater, the top heater 2 and four side heaters 4 are existing polycrystalline silicon ingot casting
Stove is identical.Each side heater 4 is in parallel laying with the side wall of crucible 1 on its inside.
Four side-wall outer sides of the crucible 1 are both provided with crucible guard boards 7, and the side heater 4 is located at crucible guard boards 7
Outside；The crucible guard boards 7 are in vertically to the graphite cake of laying.
Meanwhile 1 lower section of crucible is additionally provided with pressure pin 9.
When actual installation, the top heater 2 and four side heaters 4 are lifted on polycrystalline by lifting part
On the head cover of silicon ingot furnace 3.
In the present embodiment, the heating power all same of four side heaters 4 in step 1 and step 2；Step 1
In carry out fusing and later stage impurities removal during, inert gas is filled with into polycrystalline silicon ingot or purifying furnace 3 and by gas in polycrystalline silicon ingot or purifying furnace 3
Pressure is maintained at Q1, wherein Q1=600mbar.
In actual use, the value size of Q1 can be adjusted accordingly according to specific needs.
Meanwhile during carrying out long brilliant and synchronous impurities removal in step 2, inert gas is filled with into polycrystalline silicon ingot or purifying furnace 3 simultaneously
Air pressure in polycrystalline silicon ingot or purifying furnace 3 is maintained at Q1.
In actual use, the practical heating power of top heater 2 described in step 1 and step 2 is 70kW~90kW；
P described in step 1dmax150kW~180kW, Pcmax=220kW~260kW.
In the present embodiment, P described in step 1dmax160kW, Pcmax=240kW.It in actual use, can be according to tool
Body needs, to PdmaxAnd PcmaxValue size adjust accordingly respectively.
In the present embodiment, when being melted in step 101, include the following steps：
Step 1011, heating：The heating temperature of polycrystalline silicon ingot or purifying furnace 3 is stepped up from T1 to T2；In temperature-rise period, institute
It states air pressure in polycrystalline silicon ingot or purifying furnace 3 and is maintained at Q1；Wherein Q1=550mbar~650mbar；
In this step, the top side of the polycrystalline silicon ingot or purifying furnace 3 is than coefficient c=1；
Step 1012 is kept the temperature for the first time：By the heating and temperature control of polycrystalline silicon ingot or purifying furnace 3 in T2, and keep the temperature 4h~8h；It protects
During temperature, in the polycrystalline silicon ingot or purifying furnace 3 air pressure be maintained at Q1；
In this step, the top side of the polycrystalline silicon ingot or purifying furnace 3 is than coefficient c=1；
Step 1013 is kept the temperature for second：By the heating and temperature control of polycrystalline silicon ingot or purifying furnace 3 in T2, and keep the temperature 10h~14h；
In insulating process, in the polycrystalline silicon ingot or purifying furnace 3 air pressure be maintained at Q1；
In this step, by adjusting top heater 2 and/or the heating power of four side heaters 4, make 0.9
≤ c ＜ 1.3.
In the present embodiment, when being melted in step 101, wait for that the thickness of 1 inside bottom silicon material of crucible is 13mm~20mm
When, fusing is completed.
In actual use, when being melted in step 101, the melt method of conventional half casting process can also be used.
It in the present embodiment, is carried out in second of insulating process in step 1013, by adjusting top heater 2 and/or four
The heating power of a side heater 4, makes c gradually reduce；
Also, it is carried out in second of insulating process in step 1013, described in top heater 2 and/or four
The heating power of side heater 4, makes c be gradually decrease to 0.95 from 1.2.
In actual use, it carries out in second of insulating process, can also be heated by adjusting top in step 1013
The heating power of device 2 and/or four side heaters 4, makes c be gradually decrease to 0.9 from 1.3.
In the present embodiment, during melting later stage impurities removal in step 103, by adjusting top heater 2 and/or four institutes
The heating power for stating side heater 4, makes c continuously decrease.
Also, during melting later stage impurities removal in step 103, by adjusting top heater 2 and/or four sides
The heating power of heater 4, makes c be gradually decrease to 0.8 from 0.95.
It in actual use, can also be by adjusting top heater 2 during melting later stage impurities removal in step 103
And/or the heating power of four side heaters 4, so that c is gradually decrease to 0.8 from 1.
In the present embodiment, in the present embodiment, during melting later stage impurities removal in step 103, by adjusting top heater 2
And/or the heating power of four side heaters 4, so that c is continuously decreased.
Also, during melting later stage impurities removal in step 103, by adjusting top heater 2 and/or four sides
The heating power of heater 4, makes c be gradually decrease to 0.8 from 0.95.
It in actual use, can also be by adjusting top heater 2 during melting later stage impurities removal in step 103
And/or the heating power of four side heaters 4, so that c is gradually decrease to 0.8 from 1.
Before carrying out long brilliant and synchronous impurities removal in the present embodiment, in step 2, first by the heating temperature of polycrystalline silicon ingot or purifying furnace 3
It is down to T4, wherein T4=1420 DEG C from T3；
Also, it is 1h~2h that the heating temperature of polycrystalline silicon ingot or purifying furnace 3 is down to the temperature fall time of T4 from T3.
When carrying out long brilliant and synchronous impurities removal in step 2, include the following steps：
Step 201, length crystalline substance early period and synchronous removal of impurities：The heating temperature of polycrystalline silicon ingot or purifying furnace 3 is gradually risen into T3 from T4, and
By adjusting top heater 2 and/or the heating power of four side heaters 4, make c from c1It is gradually decrease to c0；Wherein
c1=0.8, c0=0.5；The early period length brilliant time is 12h；
Step 202, later stage length are brilliant and synchronize removal of impurities：The heating temperature of polycrystalline silicon ingot or purifying furnace 3 is gradually down to T5 from T3, and
By adjusting top heater 2 and/or the heating power of four side heaters 4, make c from c0Gradually increase to 1；Wherein T5
=1415 DEG C；The later stage length brilliant time is 31h.
During carrying out long brilliant and synchronous impurities removal in the present embodiment, in step 2, long crystalline substance rate control is in 12mm/h.
Also, during carrying out long brilliant and synchronous impurities removal in step 2, according to the long brilliant rate controlled, to putting forward cage height
It is determined.
In the present embodiment, the inert gas is argon gas.
In the present embodiment, the surface free from admixture of processed forming polycrystalline silicon ingot casting, without viscous crucible phenomenon, ingot casting bottom oxygen content
62% or more reduction, minority carrier life time ＞ 5.5us (microsecond), Hard Inclusion ratio ＜ 0.5%, yield rate 86%.
Embodiment 2
In the present embodiment, as different from Example 1：P described in step 1dmax150kW, Pcmax=220kW；Step
It T1=1125 DEG C in 101, T2=1530 DEG C, carries out in step 1012 keeping the temperature 8h when keeping the temperature for the first time, the is carried out in step 1013
14h is kept the temperature when secondary heat preservation；Q2=350mbar in step 1021, dip time 12min, in step 1022 dwell time be
60min；In step 103 continue fusing time be 40min, T3=1420 DEG C；T4=1410 DEG C in step 2, c in step 2011
=0.9, c0=0.6, the early period length brilliant time is 15h；T5=1405 DEG C in step 202, the later stage length brilliant time is 35h；Step 2
Middle long brilliant rate control is in 10mm/h；Q1=550mbar described in step 1 and step 2.
In the present embodiment, remaining method and step and technological parameter are same as Example 1.
In the present embodiment, the surface free from admixture of processed forming polycrystalline silicon ingot casting, without viscous crucible phenomenon, ingot casting bottom oxygen content
65% or more reduction, minority carrier life time ＞ 5.5us (microsecond), Hard Inclusion ratio ＜ 0.5%, yield rate 82%.
Embodiment 3
In the present embodiment, as different from Example 1：P described in step 1dmax180kW, Pcmax=260kW；Step
It T1=1285 DEG C in 101, T2=1550 DEG C, carries out in step 1012 keeping the temperature 4h when keeping the temperature for the first time, the is carried out in step 1013
10h is kept the temperature when secondary heat preservation；Q2=450mbar in step 1021, dip time 8min, in step 1022 dwell time be
10min；In step 103 continue fusing time be 15min, T3=1440 DEG C；T4=1430 DEG C in step 2, c in step 2011
=0.8, c0=0.3, the early period length brilliant time is 10h；T5=1425 DEG C in step 202, the later stage length brilliant time is 28h；Step 2
Middle long brilliant rate control is in 13mm/h；Q1=650mbar described in step 1 and step 2.
In the present embodiment, remaining method and step and technological parameter are same as Example 1.
In the present embodiment, the surface free from admixture of processed forming polycrystalline silicon ingot casting, without viscous crucible phenomenon, ingot casting bottom oxygen content
70% or more reduction, minority carrier life time ＞ 5.5us (microsecond), Hard Inclusion ratio ＜ 0.5%, yield rate 78%.
The above is only presently preferred embodiments of the present invention, is not imposed any restrictions to the present invention, every according to the present invention
Technical spirit changes any simple modification, change and equivalent structure made by above example, still falls within skill of the present invention
In the protection domain of art scheme.
Claims (9)
1. a kind of polysilicon fritting ingot casting sundries discharging method, which is characterized in that this approach includes the following steps：
Step 1: fusing and impurities removal, process are as follows：
Step 101, fusing：By the top heater (2) and four difference in polycrystalline silicon ingot or purifying furnace (3) above crucible (1)
Be laid in four side-wall outer sides of crucible (1) side heater (4) open after, according to conventional polysilicon fritting ingot casting
Method melts the silicon material being loaded in crucible (1) using polycrystalline silicon ingot or purifying furnace (3), and fusion temperature is T1~T2；Wherein, T1
=1125 DEG C~1285 DEG C, T2=1530 DEG C~1550 DEG C；
It is carried out in fusion process in step 101, to being filled with inert gas in polycrystalline silicon ingot or purifying furnace (3) and by polycrystalline silicon ingot or purifying furnace
(3) interior air pressure is maintained at Q1, wherein Q1=550mbar~650mbar；
Step 102, decompression impurities removal, process are as follows：
Step 1021, decompression：By the heating and temperature control of polycrystalline silicon ingot or purifying furnace (3) in T2, and by the gas of polycrystalline silicon ingot or purifying furnace (3)
Pressure is down to Q2 by Q1, and dip time is 8min~12min；Wherein, Q2=350mbar~450mbar；
Step 1022, pressurize：By the heating and temperature control of polycrystalline silicon ingot or purifying furnace (3) in T2, and by polycrystalline silicon ingot or purifying furnace (3) interior gas
Pressure is maintained at Q2, and the dwell time is 10min~60min；
Step 103, fusing later stage impurities removal：The air pressure of polycrystalline silicon ingot or purifying furnace (3) is first risen into Q1 by Q2, then uses polycrystalline silicon ingot casting
Stove (3) continues to melt to the silicon material being loaded in crucible (1), and continuation fusing time is 15min~40min；
Continue in fusion process, by adjusting top heater (2) and/or the heating power of four side heaters (4),
Make 0.8≤c ＜ 1, and the heating temperature of polycrystalline silicon ingot or purifying furnace (3) is made gradually to be down to T3 from T2；Wherein, T3 is polysilicon crystal temperature
Degree and T3=1420 DEG C~1440 DEG C；
Wherein, c be the top side of polycrystalline silicon ingot or purifying furnace (3) than coefficient andcdingFor the power ratio system of top heater (2)
Number andPdFor the practical heating power of top heater (2), PdmaxFor the maximum heating of top heater (2)
Power；PcFor the practical heating power of side heater (4), PcmaxFor the maximum heating work(of side heater (4)
Rate；Pdmax＜ Pcmax；
Step 2: long brilliant and synchronous impurities removal：In step 1 after the completion of fusing and impurities removal, proceeds by directional solidification and enter long brilliant
Process；During long crystalline substance, by adjusting top heater (2) and/or the heating power of four side heaters (4), make
0.3≤c ＜ 0.9；
During carrying out long brilliant and synchronous impurities removal in step 2, long crystalline substance rate control is in 10mm/h~13mm/h.
2. a kind of polysilicon fritting ingot casting sundries discharging method described in accordance with the claim 1, it is characterised in that：Described in step 1
Top heater (2) is connect by first electrode with top heating power supply (2-1), and four side heaters (4) pass through
Second electrode is connect with side heating power supply (4-1)；The top heating power supply (2-1) and side heating power supply (4-1) with
Heating power regulating device (6) connects, and the heating power regulating device (6) is to add to top heating power supply (2-1) and side
The PCU Power Conditioning Unit that the output power of thermoelectric generator (4-1) is adjusted respectively.
3. according to a kind of polysilicon fritting ingot casting sundries discharging method as claimed in claim 1 or 2, it is characterised in that：Step 1 and
The heating power all same of four side heaters (4) in step 2.
4. according to a kind of polysilicon fritting ingot casting sundries discharging method as claimed in claim 1 or 2, it is characterised in that：Step 1 and
The practical heating power of top heater described in step 2 (2) is 70kW~90kW；P described in step 1dmax150kW~
180kW, Pcmax=220kW~260kW.
5. according to a kind of polysilicon fritting ingot casting sundries discharging method as claimed in claim 1 or 2, it is characterised in that：In step 101
When being melted, include the following steps：
Step 1011, heating：The heating temperature of polycrystalline silicon ingot or purifying furnace (3) ingot furnace is stepped up from T1 to T2；Temperature-rise period
In, the interior air pressure of the polycrystalline silicon ingot or purifying furnace (3) is maintained at Q1；Wherein Q1=550mbar~650mbar；
In this step, the top side of the polycrystalline silicon ingot or purifying furnace (3) is than coefficient c=1；
Step 1012 is kept the temperature for the first time：By the heating and temperature control of polycrystalline silicon ingot or purifying furnace (3) in T2, and keep the temperature 4h~8h；Heat preservation
In the process, the interior air pressure of the polycrystalline silicon ingot or purifying furnace (3) is maintained at Q1；
In this step, the top side of the polycrystalline silicon ingot or purifying furnace (3) is than coefficient c=1；
Step 1013 is kept the temperature for second：By the heating and temperature control of polycrystalline silicon ingot or purifying furnace (3) in T2, and keep the temperature 10h~14h；It protects
During temperature, the interior air pressure of the polycrystalline silicon ingot or purifying furnace (3) is maintained at Q1；
In this step, by adjusting top heater (2) and/or the heating power of four side heaters (4), make 0.9
≤ c ＜ 1.3.
6. a kind of polysilicon fritting ingot casting sundries discharging method according to claim 5, it is characterised in that：In step 1013 into
In second of insulating process of row, by adjusting top heater (2) and/or the heating power of four side heaters (4),
C is set to be gradually decrease to 0.95 from 1.2.
7. a kind of polysilicon fritting ingot casting sundries discharging method according to claim 6, it is characterised in that：It is melted in step 103
During changing later stage impurities removal, by adjusting top heater (2) and/or the heating power of four side heaters (4), make
C is gradually decrease to 0.8 from 0.95.
8. according to a kind of polysilicon fritting ingot casting sundries discharging method as claimed in claim 1 or 2, it is characterised in that：In step 2
Before carrying out long brilliant and synchronous impurities removal, the heating temperature of polycrystalline silicon ingot or purifying furnace (3) is first down to T4, wherein T4=1410 DEG C from T3
~1430 DEG C；
When carrying out long brilliant and synchronous impurities removal in step 2, include the following steps：
Step 201, length crystalline substance early period and synchronous removal of impurities：The heating temperature of polycrystalline silicon ingot or purifying furnace (3) is gradually risen into T3 from T4, and is led to
The heating power for crossing adjustment top heater (2) and/or four side heaters (4), makes c from c1It is gradually decrease to c0；Its
Middle c1=0.8~0.9, c0=0.3~0.6；The early period length brilliant time is 10h~15h；
Step 202, later stage length are brilliant and synchronize removal of impurities：The heating temperature of polycrystalline silicon ingot or purifying furnace (3) is gradually down to T5 from T3, and is led to
The heating power for crossing adjustment top heater (2) and/or four side heaters (4), makes c from c0Gradually increase to 1；Wherein
T5=1405 DEG C~1425 DEG C；The later stage length brilliant time is 28h~35h.
9. according to a kind of polysilicon fritting ingot casting sundries discharging method as claimed in claim 1 or 2, it is characterised in that：In step 101
When being melted, when the thickness of crucible (1) inside bottom silicon material is 13mm~20mm, fusing is completed.
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