CN106087044A - A kind of polycrystalline silicon ingot casting melt method based on auxiliary heating - Google Patents
A kind of polycrystalline silicon ingot casting melt method based on auxiliary heating Download PDFInfo
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- CN106087044A CN106087044A CN201610693959.7A CN201610693959A CN106087044A CN 106087044 A CN106087044 A CN 106087044A CN 201610693959 A CN201610693959 A CN 201610693959A CN 106087044 A CN106087044 A CN 106087044A
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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 polycrystalline silicon ingot casting melt method based on auxiliary heating, including step: one, auxiliary heater is installed: install auxiliary heater in polycrystalline silicon ingot or purifying furnace, auxiliary heater is to be laid in the bottom heater below crucible, and bottom heater, top heater and four side heater form hexahedro heater；Two, charging；Three, preheating: hexahedro heater is opened, and uses polycrystalline silicon ingot or purifying furnace that the silicon material being loaded in crucible is preheated；Four, fusing, process is as follows: 401, heat up for the first time；402, second time heats up；403, subsequent melting.The inventive method step is simple, reasonable in design, it is convenient to realize and be prone to grasp, using effect good, can solve present in existing polycrystalline silicon ingot casting melt process that melting efficiency is relatively low, heats is poor, the problem such as oxygen content polycrystalline silicon ingot casting Quality Down that is higher and that cause bottom ingot casting finished product due to melt deficiency of time or melt overlong time.
Description
Technical field
The invention belongs to polycrystalline silicon ingot casting technical field, especially relate to a kind of polycrystalline silicon ingot casting based on auxiliary heating and use
Melt method.
Background technology
Photovoltaic generation is one of currently the most important clean energy resource, has great development potentiality.Restriction photovoltaic industry is sent out
The key factor of exhibition, is on the one hand that electricity conversion is low, is on the other hand high expensive.Photovoltaic silicon wafer is to produce solar-electricity
Pond and the stock of assembly, for produce photovoltaic silicon wafer polysilicon purity must (i.e. non-silicon impurity always contains more than 6N level
Amount is at below 1ppm), otherwise the performance of photovoltaic cell is by by the biggest negative effect.In recent years, polysilicon chip production technology
Having had marked improvement, polycrystalline cast ingot technology arrives from G4 (each silicon ingot weighs about 270 kilograms, can cut 4 × 4=16 silicon side) progress
G5 (5 × 5=25 silicon side) is the most progressive to G6 (6 × 6=36 silicon side).Further, 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.
In actual production process, during solar energy polycrystalline silicon ingot casting, need to use silica crucible to load silicon material, and by silicon material throw
After entering silica crucible, the most also need preheated, fusing (also referred to as melt), long brilliant (also referred to as directional solidification crystallization), annealing,
The steps such as cooling, just can complete polycrystalline silicon ingot casting process.Actual when carrying out polycrystalline silicon ingot casting, the control of melt process is the most direct
Affecting ingot casting efficiency, and can directly influence quality and the yield rate of ingot casting finished product, melt process control is bad, may cause
The defects such as viscous crucible, crystalline substance splits, purity is low, directly affect yield rate.The heater that existing polycrystalline silicon ingot or purifying furnace is used generally is
Five heating arrangements, are i.e. provided with heater at the top of crucible and four side-wall outer side, this five mode of heatings from
Upper and under carry out heat radiation, melting efficiency is relatively low, simultaneously crucible bottom gas be difficult to get rid of, make bottom ingot casting finished product is oxygen-containing
Measure higher.
Summary of the invention
The technical problem to be solved is for above-mentioned deficiency of the prior art, it is provided that a kind of based on auxiliary
The polycrystalline silicon ingot casting melt method of heating, its method step is simple, reasonable in design, it is convenient to realize and is prone to grasp, use effect
The best, can solve present in existing polycrystalline silicon ingot casting melt process that melting efficiency is relatively low, heats is poor, at the bottom of ingot casting finished product
The oxygen content in portion polycrystalline silicon ingot casting Quality Down that is higher and that cause due to melt deficiency of time or melt overlong time etc.
Problem.
For solving above-mentioned technical problem, the technical solution used in the present invention is: a kind of polysilicon casting based on auxiliary heating
Ingot melt method, it is characterised in that the method comprises the following steps:
Step one, auxiliary heater are installed: install auxiliary heater in polycrystalline silicon ingot or purifying furnace；
Described auxiliary heater is to be laid in the bottom heater below crucible, described crucible be cube crucible and its in
Level is laid, and described bottom heater, is laid in the top heater above crucible and four be laid in crucible respectively four
The side heater of side-wall outer side forms hexahedro heater；Described top heater and bottom heater are all laid in level,
Four described side heater all in vertically to laying；Described top heater, bottom heater and four described sidepiece heating
Device is all laid in polycrystalline silicon ingot or purifying furnace；
Step 2, charging: the interior crucible being loaded on silicon material is loaded in polycrystalline silicon ingot or purifying furnace；
Step 3, preheating: top heater, bottom heater and four described side heater are all opened, and uses
The silicon material being loaded in crucible is preheated by polycrystalline silicon ingot or purifying furnace, and the heating-up temperature of polycrystalline silicon ingot or purifying furnace is stepped up to
T1；Preheating time is 4h～6h, wherein T1=1125 DEG C～1285 DEG C；
Step 4, fusing, process is as follows:
Step 401, for the first time intensification: use polycrystalline silicon ingot or purifying furnace that the silicon material being loaded in crucible is melted, fusing temperature
Degree is stepped up to T2 by T1；Wherein T2=1350 DEG C～1400 DEG C；
Step 402, second time heat up: use polycrystalline silicon ingot or purifying furnace to continue to melt the silicon material being loaded in crucible, molten
Change temperature to be stepped up to T3 by T2；Wherein T3=1540 DEG C～1560 DEG C；
Step 403, subsequent melting: after the silicon material in crucible all melts, by the heating-up temperature control of polycrystalline silicon ingot or purifying furnace
System is at T3, and the heating power of the most described top heater and four described side heater all begins to decline, and treats described top
After the heating power of heater and four described side heater all stops decline and persistent period t, melt process completes；Wherein
T=20min～40min；
Top heater described in step 401, step 402 and step 403 and four described side heater are in out
Opening state, described bottom heater is closed.
A kind of above-mentioned polycrystalline silicon ingot casting melt method based on auxiliary heating, is characterized in that: warm in step 3
In neutralization procedure 401 in first time temperature-rise period, top heater, bottom heater and four described sidepieces described in synchronization
The heating power of heater is the most identical；In step 402 second time temperature-rise period neutralization procedure 403 in subsequent melting during, with
Top heater described in one moment is the most identical with the heating power of four described side heater.
A kind of above-mentioned polycrystalline silicon ingot casting melt method based on auxiliary heating, is characterized in that: warm in step 3
In, synchronize to be stepped up by the heating power of top heater, bottom heater and four described side heater, and will
The heating power of top heater, bottom heater and four described side heater is all stepped up to P1, wherein P1=
50kW～100kW；
In step 401 in first time temperature-rise period, described top heater, bottom heater and four described sidepieces heating
The heating power of device is P1；
In step 402 in second time temperature-rise period, described top heater and four described side heater add hot merit
Rate is P1；
In step 403 subsequent melting during, after the silicon material in crucible all melts, described top heater and four
The heating power of described side heater synchronizes progressively to decline, and becomes the heating power of top heater or side heater
Change situation is observed, and when the heating power of top heater or side heater drops to P2, keeps P2 constant and continues
After time t, melt process completes；Wherein, P2=25kW～45kW.
A kind of above-mentioned polycrystalline silicon ingot casting melt method based on auxiliary heating, is characterized in that: assist in step one
When heater is installed, also need all to regulate top heater, bottom heater and four described side heater with heating power
Device connects；
In step 3 in warm, use heating power adjusting means to top heater, bottom heater and four
The heating power of described side heater synchronizes to be stepped up.
A kind of above-mentioned polycrystalline silicon ingot casting melt method based on auxiliary heating, is characterized in that: described top heater is led to
Crossing the first electrode to be connected with top firing power supply, four described side heater are all by the second electrode with sidepiece heating power supply even
Connecing, described bottom heater is connected with bottom-heated power supply by the 3rd electrode；Described top firing power supply, sidepiece heating power supply
All be connected with heating power adjusting means with bottom-heated power supply, described heating power adjusting means be to top firing power supply,
The PCU Power Conditioning Unit that the output of sidepiece heating power supply and bottom-heated power supply is adjusted respectively.
A kind of above-mentioned polycrystalline silicon ingot casting melt method based on auxiliary heating, is characterized in that: preheating time in step 3
For 5h；In warm, by the heating power of polycrystalline silicon ingot or purifying furnace with the rate of rise of 10kW/h～15kW/h step up to
P1；
The heating power of described polycrystalline silicon ingot or purifying furnace is the heating power of top heater or side heater.
A kind of above-mentioned polycrystalline silicon ingot casting melt method based on auxiliary heating, is characterized in that: fusion process in step 4
In, in polycrystalline silicon ingot or purifying furnace, it is filled with noble gas and polycrystalline silicon ingot or purifying furnace internal gas pressure is maintained at Q1, wherein Q1=550mbar
～650mbar.
A kind of above-mentioned polycrystalline silicon ingot casting melt method based on auxiliary heating, is characterized in that: melt in step 4
Time, process is as follows:
1st step, insulation: by the heating and temperature control of polycrystalline silicon ingot or purifying furnace at T1, and it is incubated 0.4h～0.6h；
2nd step to the 5th step, heat up and pressurize: by first to rear point of four step by the heating-up temperature of polycrystalline silicon ingot or purifying furnace by T1 by
Gradually being promoted to T4, the heating-up time is 0.4h～0.6h；Temperature-rise period is filled with in polycrystalline silicon ingot or purifying furnace noble gas and will be many
Crystal silicon ingot furnace internal gas pressure steps up to Q1；Wherein, T4=1190 DEG C～1325 DEG C；
6th step, for the first time intensification and pressurize: the heating-up temperature of polycrystalline silicon ingot or purifying furnace is gradually promoted to by T4 T5 and intensification
Time is 3.5h～4.5h, and in temperature-rise period, polycrystalline silicon ingot or purifying furnace internal gas pressure is maintained at Q1；Wherein, T5=1440 DEG C～1460
℃；
7th step: second time heats up and pressurize: the heating-up temperature of polycrystalline silicon ingot or purifying furnace is gradually promoted to T6 and intensification by T5
Time is 3.5h～4.5h, and in temperature-rise period, polycrystalline silicon ingot or purifying furnace internal gas pressure is maintained at Q1；Wherein, T6=1490 DEG C～1510
℃；
8th step, third time heat up and pressurize: the heating-up temperature of polycrystalline silicon ingot or purifying furnace is gradually promoted to T3 and intensification by T6
Time is 3.5h～4.5h, and in temperature-rise period, polycrystalline silicon ingot or purifying furnace internal gas pressure is maintained at Q1；
9th step, insulation: by the heating and temperature control of polycrystalline silicon ingot or purifying furnace at T3, and it is incubated 3.5h～4.5h；Insulating process
In, described polycrystalline silicon ingot or purifying furnace internal gas pressure is maintained at Q1；
10th step, persistently insulation: by the heating and temperature control of polycrystalline silicon ingot or purifying furnace at T3, and be incubated 4h～8h, until earthenware
Silicon material in crucible all melts；In insulating process, described polycrystalline silicon ingot or purifying furnace internal gas pressure is maintained at Q1.
A kind of above-mentioned polycrystalline silicon ingot casting melt method based on auxiliary heating, is characterized in that: carry out in the 6th step for the first time
In intensification and pressure maintaining period, the 7th step is carried out heat up for the second time and carry out in pressure maintaining period, in the 8th step heat up and protect for the third time
Press through and Cheng Zhonghe the 9th step carry out in insulating process, be both needed to the heating power situation of change of polycrystalline silicon ingot or purifying furnace is observed,
And guarantee the heating power change of polycrystalline silicon ingot or purifying furnace steadily；
The heating power of described polycrystalline silicon ingot or purifying furnace is the heating power of top heater or side heater.
Above-mentioned a kind of based on auxiliary heating polycrystalline silicon ingot casting melt method, it is characterized in that: in the 2nd step to the 5th step by
When the heating-up temperature of described ingot furnace is gradually promoted to T4 by T1 by elder generation to rear point of four steps, each step promotes temperature 5 DEG C～8 DEG C,
And each step promotes and is both needed to 5min～10min.
The present invention compared with prior art has the advantage that
1, reasonable in design and treatment process steps is simple, it is easy to grasp.
2, input cost is low and realizes conveniently.
3, the hexahedro heater simple in construction that used, reasonable in design and input cost is relatively low, is laid in polysilicon casting
In ingot stove, and it is provided with the temperature-detecting device that the heating-up temperature to hexahedro heater detects in real time, temperature control process
Easily controllable and temperature detection result intuitive display, can be to the heating temperature of top heater, bottom heater and side heater
Degree detects the most in real time.
4, the hexahedro heater used is installed and is laid simplicity, and to existing polycrystalline silicon ingot or purifying furnace inner heating device
Change less, only need to set up bottom heater below crucible, and bottom heater is fixed on and is supported in crucible bottom
DS block on, fixing simplicity.
5, in the hexahedro heater used, top heater, bottom heater and side heater use the most independent
Power supply, top heater, bottom heater and side heater can individually control and the heating power of three can separate
Individually be controlled, now control mode have the advantage that first, more energy-conservation, as sidepiece can be reduced in crystal growing stage
The heat time heating time of heater, thus reach to reduce the purpose of h eating power, can effectively reduce unit interval inner cooling water band simultaneously
The heat walked, thus indirectly decrease the load of power refrigeration equipment；The second, thermal field can be better controled over, owing to top adds
Hot device, bottom heater and side heater can individually control, and simplicity can realize top heater, bottom heater and side
The purpose of portion's heater separately heating, it is thus possible to reach effectively to control the purpose of thermal field；3rd, crystal growing process is had
The biggest improvement result, is conducive to being internally formed vertical gradient thermal field evenly at polycrystalline silicon ingot or purifying furnace, thus preferably controls
The long brilliant speed of system so that long crystal boundary face is more mild, thus reduces the unfavorable factor such as shade, red sector, and heats is more preferably；The
Four, can effectively alleviate the load of carrying on main line, effectively reduce the electric current superposition amount on main line, thus reduce line load
Amount, has certain protective effect for bus and switchgear house；5th, the service life of internal thermal field can be extended, as on long brilliant rank
After section reduces the heat time heating time of side heater, can effectively reduce the side heater thermo-contact time to adjacent warming plate, from
And extend the service life of internal insulation plate and thermal field.
6, the hexahedro heater used uses easy and simple to handle, is added hexahedro heater by temperature-detecting device
Hot temperature detects and by detected temperature information synchronous driving in real time to main controller, then by main controller to being laid in polycrystalline
Hexahedro heater in silicon ingot furnace is controlled.
7, the hexahedro heater using effect used is good and practical value high, changes existing polycrystalline silicon ingot or purifying furnace and adopts
Carry out thermal-radiating mode of heating from top to down with five heating arrangements, after setting up bottom heater below crucible, form one
Individual from upper and lower, left and right, front and rear six direction hexahedro heating arrangement that silicon material in crucible is heated, and control letter
Just, temperature control process is easily controllable, can not only improve melting efficiency, and can be effectively improved the heating of crucible bottom during melt
Speed, beneficially crucible bottom gas are discharged, it is thus possible to effectively reduce the bottom oxygen content of ingot casting finished product, can significantly improve ingot casting
The yield rate of finished product and quality.Thus, use hexahedro heater that silicon material in crucible is heated, existing polysilicon can be solved
The melting efficiency that ingot furnace is used five heating arrangements to exist is relatively low, crucible bottom gas is difficult to bottom eliminating, ingot casting finished product
The problem such as oxygen content is higher.
8, during melt, the heating power of top heater, bottom heater and side heater controls easy and realizes
Convenient, in fusion process, after the silicon material in crucible all melts, the heating-up temperature controlling polycrystalline silicon ingot or purifying furnace keeps constant,
And the time dependent curve of heating power (i.e. power curve) of polycrystalline silicon ingot or purifying furnace is observed；Wherein, in treating crucible
Silicon material all melt after, the power curve of polycrystalline silicon ingot or purifying furnace begins to decline, treat polycrystalline silicon ingot or purifying furnace power curve decline
And after walking flat 20min～40min, melt process completes, carry out crystal growing stage afterwards.In actual mechanical process, by observation merit
Rate curve just can accurately determine the time point that melt process completes, and is i.e. switched to the switching time of crystal growing stage by the melting stage
Point.Practical operation is easy, and realizes conveniently, and energy accurate assurance is switched to the switching time of crystal growing stage by the melting stage.The most just
Being to say, the present invention stablizes ingot casting melt curve by extending the melt time, cuts after power curve walks flat 20min～40min again
Enter crystal growing stage, thus can accurately be melted to the switching time of crystal growing stage, stopped due to melt deficiency of time or molten simultaneously
Polycrystalline silicon ingot casting Quality Down that material overlong time causes, the problem such as cost increase.Further, use the present invention to polycrystalline silicon ingot casting
During after melt carries out accurate assurance to long brilliant switching time, can ensure that long brilliant quality and be finally made turning of cell piece
Change efficiency, it is to avoid because of can not accurate assurance by the melting stage be switched to that the switching time of crystal growing stage causes accordingly due to melt
Deficiency of time or melt overlong time and the problem of produced polycrystalline silicon ingot casting Quality Down that causes.
9, fusion process is divided into intensification for the first time, second time to rise gentle subsequent melting three key steps, and mode of heating sets
Rationally, heating power is separately individually controlled meter, and not only control simplicity and heats more preferably, can be effectively improved melt process
The rate of heat addition of middle crucible bottom, beneficially crucible bottom gas are discharged, it is thus possible to the bottom oxygen effectively reducing ingot casting finished product contains
Amount, can significantly improve yield rate and the quality of ingot casting finished product；Meanwhile, can be to melt during polycrystalline silicon ingot casting to long brilliant switching
Opportunity carries out accurate assurance, can be effectively improved crystal growth quality, reduces viscous crucible rate, improves the conversion efficiency of solar battery sheet, energy
It is effectively improved yield rate.
Further, warm uses hexahedro heating, and fusion process all uses roofing to heat, and main reason is that and prevents silicon
Become bottom material after liquid with coating reaction, cause the phenomenons such as viscous pot, crystalline substance split.
10, practical, it is simple to batch production and widely applicable, the present invention is applicable to the melt mistake of fine melt ingot casting method
Journey.
In sum, the inventive method step is simple, reasonable in design, it is convenient to realize and be prone to grasp, using effect good, energy
Effectively solve present in existing polycrystalline silicon ingot casting melt process that melting efficiency is relatively low, heats is poor, bottom ingot casting finished product
Oxygen content produced polycrystalline silicon ingot casting quality that is higher and that cause due to melt deficiency of time or melt overlong time under
Degradation problem.
Below by drawings and Examples, technical scheme is described in further detail.
Accompanying drawing explanation
Fig. 1 is the method flow block diagram of the present invention.
Fig. 2 is used the use view of hexahedro heater by the present invention.
Fig. 3 is used the schematic block circuit diagram of hexahedro heater by the present invention.
Fig. 4 is temperature and the power curve using the present invention to carry out top heater and side heater during polycrystalline silicon ingot casting
Figure.
Description of reference numerals:
1 crucible；2 top heater；2-1 top firing power supply；
3 bottom heaters；3-1 bottom-heated power supply；4 side heater；
4-1 sidepiece heating power supply；5 DS blocks；6 heating power adjusting meanss；
7 crucible guard boards；8 main controllers；9 polycrystalline silicon ingot or purifying furnaces；
10 top firing temperature detecting units；
11 sidepiece heating-up temperature detector units；
12 bottom-heated temperature detecting units；13 heat-preservation cylinders；
14 pressure pins；15 display units；16 parameter set unit.
Detailed description of the invention
Embodiment 1
A kind of based on auxiliary heating polycrystalline silicon ingot casting melt method as shown in Figure 1, comprises the following steps:
Step one, auxiliary heater are installed: install auxiliary heater in polycrystalline silicon ingot or purifying furnace 9；
Described auxiliary heater is to be laid in the bottom heater 3 below crucible 1, described crucible 1 be cube crucible and
It is level lay, described bottom heater 3, be laid in the top heater 2 above crucible 1 and four be laid in crucible respectively
The side heater 4 of four side-wall outer side of 1 forms hexahedro heater；Described top heater 2 and bottom heater 3 all in
Level is laid, four described side heater 4 all in vertically to laying；Described top heater 2, bottom heater 3 and four
Described side heater 4 is all laid in polycrystalline silicon ingot or purifying furnace 9, refers to Fig. 2；
Step 2, charging: the interior crucible 1 being loaded on silicon material is loaded in polycrystalline silicon ingot or purifying furnace 9；
Step 3, preheating: top heater 2, bottom heater 3 and four described side heater 4 are all opened, and adopts
With polycrystalline silicon ingot or purifying furnace 9, the silicon material being loaded in crucible 1 is preheated, and the heating-up temperature of polycrystalline silicon ingot or purifying furnace 9 is progressively carried
Rise to T1；Preheating time is 5h, wherein T1=1200 DEG C；
Step 4, fusing, process is as follows:
Step 401, for the first time intensification: use polycrystalline silicon ingot or purifying furnace 9 that the silicon material being loaded in crucible 1 is melted, fusing
Temperature is stepped up to T2 by T1；Wherein T2=1380 DEG C；
Step 402, second time heat up: the silicon material using polycrystalline silicon ingot or purifying furnace 9 to continue being loaded in crucible 1 melts,
Fusion temperature is stepped up to T3 by T2；Wherein T3=1550 DEG C；
Step 403, subsequent melting: after the silicon material in crucible 1 all melts, by the heating-up temperature of polycrystalline silicon ingot or purifying furnace 9
Controlling at T3, the heating power of the most described top heater 2 and four described side heater 4 all begins to decline, and treats described
After the heating power of top heater 2 and four described side heater 4 all stops decline and persistent period t, melt process is complete
Become (i.e. fusion process completes)；Wherein t=30min.
Top heater 2 described in step 401, step 402 and step 403 and four described side heater 4 are in
Opening, described bottom heater 3 is closed.
At present, polycrystalline silicon ingot casting method mainly has half casting process and fine melt ingot casting method two kinds, and half casting process is also referred to as
There is seed crystal ingot casting polycrystalline silicon process, refer to use grade silicon material to carry out epitaxial growth as nucleating center, cast low defect Gao Pin
The polycrystalline silicon ingot casting of matter；Fine melt ingot casting method is also referred to as without seed crystal ingot casting polycrystalline silicon process or without seed crystal efficient polycrystalline silicon technology, refers to
Non-silicon material is used to prepare shaggy heterogeneous forming core layer bottom crucible 1, by controlling roughness and the forming core of forming core layer
Time degree of supercooling obtain bigger nucleation rate, cast low defect high-quality polycrystalline silicon ingot casting.At present, polycrystalline silicon ingot casting method is with fine melt
Ingot casting method is main.In the present embodiment, when step 2 feeds, fill according to the loading method of conventional fine melt ingot casting method
Material.
In the present embodiment, polycrystalline silicon ingot or purifying furnace 9 described in step 2 is G5 type ingot furnace.Further, described polycrystalline silicon ingot casting
Stove 9 is specially the G5 type ingot furnace that Zhejiang Jingsheng Electrical and Mechanical Co., Ltd. produces.Described crucible 1 be silica crucible and its be G5
Crucible, and the polycrystalline silicon ingot casting produced is G5 ingot.
Time actually used, the charge of described silica crucible is about 600kg.
In the present embodiment, the charge of described silica crucible is 560kg.During actually used, can be according to concrete need
Want, the charge of described silica crucible is adjusted accordingly.
In conjunction with Fig. 3, in the present embodiment, when step one carries out auxiliary heater installation, also need top heater 2, the end
Portion's heater 3 and four described side heater 4 are all connected with heating power adjusting means 6；
In step 3 in warm, use heating power adjusting means 6 to top heater 2, bottom heater 3 and four
The heating power of individual described side heater 4 synchronizes to be stepped up.
In the present embodiment, hexahedro heater described in step one also includes main controller 8 and temperature-detecting device, described temperature
Top firing temperature detecting unit 10 that degree detection device includes detecting the heating-up temperature of top heater 2 in real time, right
Sidepiece heating-up temperature detector unit 11 that the heating-up temperature of side heater 4 detects in real time and adding bottom heater 3
The bottom-heated temperature detecting unit 12 that hot temperature detects in real time, described top firing temperature detecting unit 10, sidepiece add
Hot temperature detecting unit 11 and bottom-heated temperature detecting unit 12 are all connected with main controller 8；Set in described polycrystalline silicon ingot or purifying furnace 9
Being equipped with heat-preservation cylinder 13, described hexahedro heater is positioned at heat-preservation cylinder 13.Meanwhile, described main controller 8 arranges list with parameter respectively
Unit 16 and display unit 15 connect.
In the present embodiment, described bottom heater 3 is fixed on the DS block 5 being supported in bottom crucible 1, described bottom-heated
Distance between bottom device 3 top and DS block 5 is 0.5cm～3cm.
During actual installation, can according to specific needs the distance between bottom bottom heater 3 top and DS block 5 be carried out
Corresponding regulation.
Wherein, DS block 5 is graphite block, and the heat conductivity of described graphite block is the strongest.Described DS block 5 also referred to as directional solidification block or
DS-BLOCK。
In the present embodiment, described heating power adjusting means 6 is connected with main controller 8.
Described top firing power supply 2-1, sidepiece heating power supply 4-1 and bottom-heated power supply 3-1 are power adjustable economize on electricity
Source, and top heater 2, bottom heater 3 be respectively adopted three different power supplys (i.e. with four described side heater 4
Described top firing power supply, described sidepiece heating power supply and described bottom-heated power supply), top heater 2 can be realized, bottom adds
Hot device 3 and the independent control of side heater 4, use easy and simple to handle and using effect good.
In the present embodiment, described heating power adjusting means 6 includes three heating power regulation equipment, adds described in three
Thermal power regulation equipment is respectively the first heating power regulation equipment, right being adjusted the heating power of top heater 2
The second heating power that the heating power of bottom heater 3 is adjusted regulates equipment and to four described side heater 4
Heating power carries out the 3rd heating power regulation equipment of adjusted in concert.
Time actually used, three described heating power regulation equipment can also share a described heating power regulation and set
Standby, only need the purpose that can reach three described power supplys are respectively controlled.
In the present embodiment, described bottom heater 3 is positioned at the underface of crucible 1.
In the present embodiment, described top heater 2, side heater 4 and bottom heater 3 are resistance heater.
Wherein, described top heater 2 and side heater 4 are the existing heating that existing polycrystalline silicon ingot or purifying furnace uses
Device, described top heater 2 and the structure of four described side heater 4 and installation position are existing polycrystalline silicon ingot or purifying furnace phase
With.Each described side heater 4 all sidewalls with crucible 1 on its inside are parallel laying.
In the present embodiment, the resistance wire material of described bottom heater 3 is the alloy cpds such as Ni, Cr, Mn.
In the present embodiment, four side-wall outer side of described crucible 1 are provided with crucible guard boards 7, described side heater 4
Outside crucible guard boards 7；Described crucible guard boards 7 is in vertically to the graphite cake laid.
Meanwhile, it is additionally provided with pressure pin 14 below described crucible 1.
During actual installation, described top heater 2 and four described side heater 4 are all lifted on polycrystalline by lifting part
On the top cover of silicon ingot furnace 9.
In the present embodiment, in step 3 in warm neutralization procedure 401 in first time temperature-rise period, described in synchronization
Top heater 2, bottom heater 3 are the most identical with the heating power of four described side heater 4；Second time in step 402
In temperature-rise period neutralization procedure 403 subsequent melting during, top heater 2 described in synchronization and the heating of four described sidepieces
The heating power of device 4 is the most identical.
In step 3 in warm neutralization procedure 401 in first time temperature-rise period, top heater described in synchronization
2, bottom heater 3 is the most identical with the heating-up temperature of four described side heater 4；In step 402 in second time temperature-rise period
With in step 403 subsequent melting during, top heater 2 described in synchronization and the heating of four described side heater 4
Temperature is the most identical.
Further, heating-up temperature or the fusion temperature of described polycrystalline silicon ingot or purifying furnace 9 is top heater 2 or side heater 4
Heating-up temperature.
In the present embodiment, in step 3 in warm, by top heater 2, bottom heater 3 and four described sidepieces
The heating power of heater 4 synchronizes to be stepped up, and top heater 2, bottom heater 3 and four described sidepieces is added
The heating power of hot device 4 is all stepped up to P1, wherein P1=75kW.
In the present embodiment, in step 3, preheating time is 5h；In warm, by the heating power of polycrystalline silicon ingot or purifying furnace 9
Step up to P1 with the rate of rise of 10kW/h～15kW/h；
The heating power of described polycrystalline silicon ingot or purifying furnace 9 is top heater 2 or the heating power of side heater 4.
Actual when preheating, can according to specific needs, to the growth speed of heating power in preheating time, warm
The value size of rate and T1 and P1 adjusts accordingly.
When step 4 melts, can according to specific needs the value size of T2, T3 and t be carried out respectively accordingly
Adjust.
In the present embodiment, in step 401 in first time temperature-rise period, described top heater 2, bottom heater 3 and four
The heating power of individual described side heater 4 is P1；
In step 402 in second time temperature-rise period, described top heater 2 and the heating of four described side heater 4
Power is P1；
In step 403 subsequent melting during, after the silicon material in crucible 1 all melts, described top heater 2 and four
The heating power of individual described side heater 4 synchronizes progressively to decline, to top heater 2 or the heating of side heater 4
Changed power situation is observed, and when the heating power of top heater 2 or side heater 4 drops to P2, keeps P2 not
Become and after persistent period t, melt process completes；Wherein, P2=35kW.
Actual when melting, according to the difference of charge in crucible 1, the size of P2 is accordingly in the range of 25kW～45kW
It is adjusted.
In the present embodiment, in step 4 in fusion process, in polycrystalline silicon ingot or purifying furnace 9, it is filled with noble gas and by polysilicon
Ingot furnace 9 internal gas pressure is maintained at Q1, wherein Q1=600mbar.
Actual when melting, can according to specific needs the value size of Q1 be adjusted accordingly.
, step 3 is carried out in warm meanwhile, in polycrystalline silicon ingot or purifying furnace 9, be filled with noble gas and polysilicon is cast
Ingot stove 9 internal gas pressure is maintained at Q1.
In the present embodiment, after the silicon material in crucible 1 all melts, the heating and temperature control of polycrystalline silicon ingot or purifying furnace 9 is existed
T3, and the time dependent curve of heating power (i.e. power curve) of polycrystalline silicon ingot or purifying furnace 9 is observed, refer to Fig. 4.Figure
In 4, fine line is the time dependent curve of heating power of polycrystalline silicon ingot or purifying furnace 9, and needing solid line is adding of polycrystalline silicon ingot or purifying furnace 9
The time dependent curve of hot temperature, vertical line is alarming line when all melting of the silicon material in crucible 1.As seen from Figure 4, treat
After silicon material in crucible 1 all melts, the power curve of described polycrystalline silicon ingot or purifying furnace 9 begins to decline, and treats polycrystalline silicon ingot or purifying furnace 9
After power curve declines and walks flat 30min, melt process completes, and enters crystal growing stage afterwards；A point in i.e. Fig. 4 is melt mistake
The time point that journey completes.
In the present embodiment, when carrying out long crystalline substance, after first the heating-up temperature of polycrystalline silicon ingot or purifying furnace 9 being gradually decreased to T7 by T3, open
Beginning be oriented solidification and enter long brilliant process, wherein T7 is polysilicon crystal temperature and T7=1420 DEG C～1440 DEG C.
In actual mechanical process, just can accurately be determined the time point that melt process completes by observed power curve, i.e. by
Melting stage is switched to some switching time of crystal growing stage.Practical operation is easy, and realizes conveniently, and energy accurate assurance is by melting rank
Section is switched to the switching time of crystal growing stage.
In the present embodiment, when melting in step 4, process is as follows:
1st step, insulation: by the heating and temperature control of polycrystalline silicon ingot or purifying furnace 9 at T1, and be incubated 0.5h；
2nd step to the 5th step, heat up and pressurize: by first to rear point of four step by the heating-up temperature of polycrystalline silicon ingot or purifying furnace 9 by T1 by
Gradually being promoted to T4, the heating-up time is 0.5h (total time of the i.e. the 2nd step to the 5th step is 0.5h)；Temperature-rise period is cast to polysilicon
It is filled with noble gas in ingot stove 9 and polycrystalline silicon ingot or purifying furnace 9 internal gas pressure is stepped up to Q1；Wherein, T4=1250 DEG C；
6th step, for the first time intensification and pressurize: the heating-up temperature of polycrystalline silicon ingot or purifying furnace 9 is gradually promoted to by T4 T5 and liter
The temperature time is 4h, and in temperature-rise period, polycrystalline silicon ingot or purifying furnace 9 internal gas pressure is maintained at Q1；Wherein, T5=1450 DEG C；
7th step: second time heats up and pressurize: the heating-up temperature of polycrystalline silicon ingot or purifying furnace 9 is gradually promoted to T6 and liter by T5
The temperature time is 4h, and in temperature-rise period, polycrystalline silicon ingot or purifying furnace 9 internal gas pressure is maintained at Q1；Wherein, T6=1500 DEG C；
8th step, third time heat up and pressurize: the heating-up temperature of polycrystalline silicon ingot or purifying furnace 9 is gradually promoted to T3 and liter by T6
The temperature time is 4h, and in temperature-rise period, polycrystalline silicon ingot or purifying furnace 9 internal gas pressure is maintained at Q1；
9th step, insulation: by the heating and temperature control of polycrystalline silicon ingot or purifying furnace 9 at T3, and be incubated 4h；In insulating process, described
Polycrystalline silicon ingot or purifying furnace 9 internal gas pressure is maintained at Q1；
10th step, persistently insulation: by the heating and temperature control of polycrystalline silicon ingot or purifying furnace 9 at T3, and be incubated 6h, until crucible 1
Interior silicon material all melts；In insulating process, described polycrystalline silicon ingot or purifying furnace 9 internal gas pressure is maintained at Q1.
In the present embodiment, by rear point of four steps by the heating-up temperature of described ingot furnace by T1 the most gradually in the 2nd step to the 5th step
When being promoted to T4, each step promotes temperature 5 DEG C～8 DEG C, and each step promotes and is both needed to 5min～10min.
In the present embodiment, the 6th step is carried out heat up for the first time and carry out in pressure maintaining period, in the 7th step second time heat up and
Carry out third time in pressure maintaining period, in the 8th step heat up and pressure maintaining period neutralization the 9th step carries out in insulating process, be both needed to many
The heating power situation of change of crystal silicon ingot furnace 9 is observed, and guarantees the heating power change of polycrystalline silicon ingot or purifying furnace 9 steadily.
The heating power of described polycrystalline silicon ingot or purifying furnace 9 is top heater 2 or the heating power of side heater 4.
During it is to say, the 6th step to the 9th step melts, it is necessary to make power curve steadily advance, it is impossible to occur more
Significantly sags and crests, so can bring increasing of Hard Inclusion.
In the present embodiment, when heating up and pressurize in the 2nd step to the 5th step, process is as follows:
2nd step, the first step promote: by 1200 DEG C, the heating-up temperature of polycrystalline silicon ingot or purifying furnace 9 is promoted to 1220 DEG C, and heat up
Time is 7min.
3rd step, second step promote: by 1220 DEG C, the heating-up temperature of polycrystalline silicon ingot or purifying furnace 9 is promoted to 1235 DEG C, and heat up
Time is 8min.
4th step, the 3rd step promote: by 1235 DEG C, the heating-up temperature of polycrystalline silicon ingot or purifying furnace 9 is promoted to 1242 DEG C, and heat up
Time is 5min.
5th step, the 4th step promote: by 1242 DEG C, the heating-up temperature of polycrystalline silicon ingot or purifying furnace 9 is promoted to 1250 DEG C, and heat up
Time is 5min.
In the present embodiment, the 10th step is treated the silicon material in crucible 1 all melt and described ingot furnace send " fusing complete report
Alert " after, need manual intervention, the decline situation of power curve is observed, treat that the power curve of described ingot furnace declines and walks
After flat 30min, melt process completes, and manual intervention afterwards will be cut into crystal growing stage the melting stage.
In the present embodiment, noble gas described in step 4 is argon.
In the present embodiment, the surface free from admixture of processed forming polycrystalline silicon ingot casting, without viscous crucible phenomenon, oxygen content bottom ingot casting
Reducing by more than 60%, minority carrier life time ＞ 5.5us (microsecond), Hard Inclusion ratio ＜ 0.5%, yield rate is 82%.
Embodiment 2
In the present embodiment, as different from Example 1: in step 3, preheating time is 4h and T1=1285 DEG C, P1=
100kW；In step 401 T2=1400 DEG C, in step 402 T3=1560 DEG C, t=20min, P2=45kW in step 403；Step
Q1=650mbar in four；In 1st step, temperature retention time is 0.4h；In 2nd step to the 5th step T4=1190 DEG C, the heating-up time is
0.4h；In 6th step, T5=1460 DEG C and heating-up time are 3.5h；In 7th step, T6=1510 DEG C and heating-up time are 3.5h；8th
In step, T3=1560 DEG C and heating-up time are 3.5h；In 9th step, temperature retention time is 3.5h；In 10th step, temperature retention time is 4h.
In the present embodiment, when heating up and pressurize in the 2nd step to the 5th step, process is as follows:
2nd step, the first step promote: by 1125 DEG C, the heating-up temperature of polycrystalline silicon ingot or purifying furnace 9 is promoted to 1140 DEG C, and heat up
Time is 9min.
3rd step, second step promote: by 1140 DEG C, the heating-up temperature of polycrystalline silicon ingot or purifying furnace 9 is promoted to 1155 DEG C, and heat up
Time is 8min.
4th step, the 3rd step promote: by 1155 DEG C, the heating-up temperature of polycrystalline silicon ingot or purifying furnace 9 is promoted to 1175 DEG C, and heat up
Time is 10min.
5th step, the 4th step promote: by 1175 DEG C, the heating-up temperature of polycrystalline silicon ingot or purifying furnace 9 is promoted to 1190 DEG C, and heat up
Time is 9min.
In the present embodiment, remaining processing step and technological parameter are the most same as in Example 1.
In the present embodiment, the surface free from admixture of processed forming polycrystalline silicon ingot casting, without viscous crucible phenomenon, oxygen content bottom ingot casting
Reducing by more than 55%, minority carrier life time ＞ 5.5us (microsecond), Hard Inclusion ratio ＜ 0.5%, yield rate is 78%.
Embodiment 3
In the present embodiment, as different from Example 1: in step 3, preheating time is 6h and T1=1125 DEG C, P1=
50kW, P2=25kW；In step 401 T2=1350 DEG C, in step 402 T3=1540 DEG C, t=40min in step 403；Step
Q1=550mbar in four；In 1st step, temperature retention time is 0.6h；In 2nd step to the 5th step T4=1325 DEG C, the heating-up time is
0.6h；In 6th step, T5=1440 DEG C and heating-up time are 4.5h；In 7th step, T6=1490 DEG C and heating-up time are 4.5h；8th
In step, T3=1540 DEG C and heating-up time are 4.5h；In 9th step, temperature retention time is 4.5h；In 10th step, temperature retention time is 8h.
In the present embodiment, when heating up and pressurize in the 2nd step to the 5th step, process is as follows:
2nd step, the first step promote: by 1285 DEG C, the heating-up temperature of polycrystalline silicon ingot or purifying furnace 9 is promoted to 1290 DEG C, and heat up
Time is 5min.
3rd step, second step promote: by 1290 DEG C, the heating-up temperature of polycrystalline silicon ingot or purifying furnace 9 is promoted to 1295 DEG C, and heat up
Time is 5min.
4th step, the 3rd step promote: by 1295 DEG C, the heating-up temperature of polycrystalline silicon ingot or purifying furnace 9 is promoted to 1315 DEG C, and heat up
Time is 9min.
5th step, the 4th step promote: by 1315 DEG C, the heating-up temperature of polycrystalline silicon ingot or purifying furnace 9 is promoted to 1325 DEG C, and heat up
Time is 5min.
In the present embodiment, remaining processing step and technological parameter are the most same as in Example 1.
In the present embodiment, the surface free from admixture of processed forming polycrystalline silicon ingot casting, without viscous crucible phenomenon, oxygen content bottom ingot casting
Reducing by more than 62%, minority carrier life time ＞ 5.5us (microsecond), Hard Inclusion ratio ＜ 0.5%, yield rate is 75%.
The above, be only presently preferred embodiments of the present invention, not impose any restrictions the present invention, every according to the present invention
Any simple modification, change and the equivalent structure change that above example is made by technical spirit, all still falls within skill of the present invention
In the protection domain of art scheme.
Claims (10)
1. a polycrystalline silicon ingot casting melt method based on auxiliary heating, it is characterised in that the method comprises the following steps:
Step one, auxiliary heater are installed: install auxiliary heater in polycrystalline silicon ingot or purifying furnace (9)；
Described auxiliary heater is the bottom heater (3) being laid in crucible (1) lower section, and described crucible (1) is cube crucible
And it is that level is laid, described bottom heater (3), the top heater (2) being laid in crucible (1) top and four difference cloth
The side heater (4) of four side-wall outer side being located at crucible (1) forms hexahedro heater；Described top heater (2) and
Bottom heater (3) is all laid in level, four described side heater (4) all in vertically to laying；Described top heater
(2), bottom heater (3) and four described side heater (4) are all laid in polycrystalline silicon ingot or purifying furnace (9)；
Step 2, charging: the interior crucible (1) being loaded on silicon material is loaded in polycrystalline silicon ingot or purifying furnace (9)；
Step 3, preheating: top heater (2), bottom heater (3) and four described side heater (4) are all opened, and
Use polycrystalline silicon ingot or purifying furnace (9) that the silicon material being loaded in crucible (1) is preheated, and by the heating temperature of polycrystalline silicon ingot or purifying furnace (9)
Degree steps up to T1；Preheating time is 4h～6h, wherein T1=1125 DEG C～1285 DEG C；
Step 4, fusing, process is as follows:
Step 401, for the first time intensification: use polycrystalline silicon ingot or purifying furnace (9) that the silicon material being loaded in crucible (1) is melted, fusing
Temperature is stepped up to T2 by T1；Wherein T2=1350 DEG C～1400 DEG C；
Step 402, second time heat up: use polycrystalline silicon ingot or purifying furnace (9) to continue to melt the silicon material being loaded in crucible (1),
Fusion temperature is stepped up to T3 by T2；Wherein T3=1540 DEG C～1560 DEG C；
Step 403, subsequent melting: after the silicon material in crucible (1) all melts, by the heating-up temperature of polycrystalline silicon ingot or purifying furnace (9)
Controlling at T3, the heating power of the most described top heater (2) and four described side heater (4) all begins to decline, and treats
The heating power of described top heater (2) and four described side heater (4) all stops declining and after persistent period t, molten
Material process completes；Wherein t=20min～40min；
Top heater described in step 401, step 402 and step 403 (2) and four described side heater (4) are in
Opening, described bottom heater (3) is closed.
2. according to a kind of based on auxiliary heating the polycrystalline silicon ingot casting melt method described in claim 1, it is characterised in that: step
In rapid three in warm neutralization procedure 401 in first time temperature-rise period, top heater described in synchronization (2), bottom add
Hot device (3) is the most identical with the heating power of four described side heater (4)；In step 402 second time temperature-rise period in and step
In rapid 403 subsequent melting during, top heater described in synchronization (2) and the heating of four described side heater (4)
Power is the most identical.
3., according to a kind of based on auxiliary heating the polycrystalline silicon ingot casting melt method described in claim 1 or 2, its feature exists
In: in step 3 in warm, by top heater (2), bottom heater (3) and four described side heater (4)
Heating power synchronizes to be stepped up, and by top heater (2), bottom heater (3) and four described side heater
(4) heating power is all stepped up to P1, wherein P1=50kW～100kW；
In step 401 in first time temperature-rise period, described top heater (2), bottom heater (3) and four described sidepieces add
The heating power of hot device (4) is P1；
In step 402 in second time temperature-rise period, described top heater (2) and the heating of four described side heater (4)
Power is P1；
In step 403 subsequent melting during, after the silicon material in crucible (1) all melts, described top heater (2) and four
The heating power of individual described side heater (4) synchronizes progressively to decline, to top heater (2) or side heater (4)
Heating power situation of change be observed, treat that the heating power of top heater (2) or side heater (4) drops to P2
Time, keep P2 constant and after persistent period t, melt process completes；Wherein, P2=25kW～45kW.
4. according to a kind of based on auxiliary heating the polycrystalline silicon ingot casting melt method described in claim 3, it is characterised in that: step
When carrying out auxiliary heater installation in rapid one, also need to add top heater (2), bottom heater (3) and four described sidepieces
Hot device (4) is all connected with heating power adjusting means (6)；
In step 3 in warm, use heating power adjusting means (6) to top heater (2), bottom heater (3) and
The heating power of four described side heater (4) synchronizes to be stepped up.
5. according to a kind of based on auxiliary heating the polycrystalline silicon ingot casting melt method described in claim 4, it is characterised in that: institute
Stating top heater (2) to be connected with top firing power supply (2-1) by the first electrode, four described side heater (4) are the most logical
Crossing the second electrode to be connected with sidepiece heating power supply (4-1), described bottom heater (3) is by the 3rd electrode and bottom-heated power supply
(3-1) connect；Described top firing power supply (2-1), sidepiece heating power supply (4-1) and bottom-heated power supply (3-1) all with heating
PCU Power Conditioning Unit (6) connects, and described heating power adjusting means (6) is to top firing power supply (2-1), sidepiece heating power supply
(4-1) PCU Power Conditioning Unit that the output with bottom-heated power supply (3-1) is adjusted respectively.
6. according to a kind of based on auxiliary heating the polycrystalline silicon ingot casting melt method described in claim 3, it is characterised in that: step
In rapid three, preheating time is 7h；In warm, by the heating power of polycrystalline silicon ingot or purifying furnace (9) with the increasing of 10kW/h～15kW/h
Long speed steps up to P1；
The heating power of described polycrystalline silicon ingot or purifying furnace (9) is top heater (2) or the heating power of side heater (4).
7., according to a kind of based on auxiliary heating the polycrystalline silicon ingot casting melt method described in claim 1 or 2, its feature exists
In: in step 4 in fusion process, in polycrystalline silicon ingot or purifying furnace (9), it is filled with noble gas and by gas in polycrystalline silicon ingot or purifying furnace (9)
Pressure is maintained at Q1, wherein Q1=550mbar～650mbar.
8. according to a kind of based on auxiliary heating the polycrystalline silicon ingot casting melt method described in claim 7, it is characterised in that: step
When melting in rapid four, process is as follows:
1st step, insulation: by the heating and temperature control of polycrystalline silicon ingot or purifying furnace (9) at T1, and be incubated 0.4h～0.6h；
2nd step to the 5th step, heat up and pressurize: by first to rear point of four steps by the heating-up temperature of polycrystalline silicon ingot or purifying furnace (9) by T1 the most gradually
Being promoted to T4, the heating-up time is 0.4h～0.6h；Temperature-rise period is filled with noble gas in polycrystalline silicon ingot or purifying furnace (9) and will be many
Crystal silicon ingot furnace (9) internal gas pressure steps up to Q1；Wherein, T4=1190 DEG C～1325 DEG C；
6th step, for the first time intensification and pressurize: the heating-up temperature of polycrystalline silicon ingot or purifying furnace (9) is gradually promoted to by T4 T5 and intensification
Time is 3.5h～4.5h, and in temperature-rise period, polycrystalline silicon ingot or purifying furnace (9) internal gas pressure is maintained at Q1；Wherein, T5=1440 DEG C～
1460℃；
7th step: second time heats up and pressurize: the heating-up temperature of polycrystalline silicon ingot or purifying furnace (9) is gradually promoted to T6 and intensification by T5
Time is 3.5h～4.5h, and in temperature-rise period, polycrystalline silicon ingot or purifying furnace (9) internal gas pressure is maintained at Q1；Wherein, T6=1490 DEG C～
1510℃；
Further, when the heating-up temperature of polycrystalline silicon ingot or purifying furnace (9) is promoted to T2, bottom heater (3) is closed；
8th step, third time heat up and pressurize: the heating-up temperature of polycrystalline silicon ingot or purifying furnace (9) is gradually promoted to T3 and intensification by T6
Time is 3.5h～4.5h, and in temperature-rise period, polycrystalline silicon ingot or purifying furnace (9) internal gas pressure is maintained at Q1；
9th step, insulation: by the heating and temperature control of polycrystalline silicon ingot or purifying furnace (9) at T3, and be incubated 3.5h～4.5h；Insulating process
In, described polycrystalline silicon ingot or purifying furnace (9) internal gas pressure is maintained at Q1；
10th step, persistently insulation: by the heating and temperature control of polycrystalline silicon ingot or purifying furnace (9) at T3, and be incubated 4h～8h, until crucible
(1) the silicon material in all melts；In insulating process, described polycrystalline silicon ingot or purifying furnace (9) internal gas pressure is maintained at Q1.
9. according to a kind of based on auxiliary heating the polycrystalline silicon ingot casting melt method described in claim 8, it is characterised in that: the
6 steps carry out heating up for the first time and carry out in pressure maintaining period, in the 7th step second time heat up and in pressure maintaining period, the 8th step is carried out
Third time heats up and pressure maintaining period neutralizes and carries out in insulating process in the 9th step, is both needed to the heating power to polycrystalline silicon ingot or purifying furnace (9)
Situation of change is observed, and guarantees the heating power change of polycrystalline silicon ingot or purifying furnace (9) steadily；
The heating power of described polycrystalline silicon ingot or purifying furnace (9) is top heater (2) or the heating power of side heater (4).
10. according to a kind of based on auxiliary heating the polycrystalline silicon ingot casting melt method described in claim 8, it is characterised in that:
When gradually the heating-up temperature of described ingot furnace being promoted to T4 by T1 by elder generation to rear point of four steps in the 2nd step to the 5th step, each step carries
Rise temperature 5 DEG C～8 DEG C, and each step promotes and is both needed to 5min～10min.
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| CN106435726A (en) * | 2016-11-17 | 2017-02-22 | 江苏美科硅能源有限公司 | Material melting process for ingot casting of polycrystal furnace |
| CN107130296A (en) * | 2017-05-03 | 2017-09-05 | 四川欣蓝光电科技有限公司 | A kind of polycrystalline silicon manufacture craft |
| CN107815727A (en) * | 2017-11-16 | 2018-03-20 | 浙江晶盛机电股份有限公司 | A kind of quick material mechanism for single crystal growing furnace |
| CN109680331A (en) * | 2019-01-21 | 2019-04-26 | 安徽华顺半导体发展有限公司 | A kind of casting ingot method of low defect polysilicon |
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