CN103741214B - A kind of polycrystalline silicon casting ingot process - Google Patents
A kind of polycrystalline silicon casting ingot process Download PDFInfo
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- CN103741214B CN103741214B CN201410041955.1A CN201410041955A CN103741214B CN 103741214 B CN103741214 B CN 103741214B CN 201410041955 A CN201410041955 A CN 201410041955A CN 103741214 B CN103741214 B CN 103741214B
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Abstract
The invention discloses a kind of polycrystalline silicon casting ingot process, comprise step: one, preheating; Two, melt; Three, long brilliant: temperature controls at T6 and is incubated 1h, T6=1420 DEG C; Heat-insulation cage lift height is 90mm; Temperature controls at T6 and is incubated 2h, and heat-insulation cage lift height is constant; Temperature controls at T6 and is incubated 3h, and heat-insulation cage lift height is 110mm; Temperature is down to T7 gradually by T6, and temperature fall time is 7 ~ 9h, and heat-insulation cage lift height is 210mm; T7=1405 DEG C; Temperature controls at T7 and is incubated 7 ~ 9h, and heat-insulation cage lift height is constant; Temperature controls at T7 and is incubated 7 ~ 9h, and heat-insulation cage lift height is constant; Temperature is down to T8 gradually by T7, and heat-insulation cage lift height is constant; T8=1395 DEG C; Four, annealing and cooling.Step of the present invention is simple, reasonable in design, it is convenient to realize and be easy to grasp, result of use is good, can carry out conservative control to the long brilliant process of ingot casting.
Description
Technical field
The invention belongs to polycrystalline silicon ingot casting technical field, especially relate to a kind of polycrystalline silicon casting ingot process.
Background technology
Photovoltaic generation is one of current most important clean energy, has great development potentiality.The key factor of restriction photovoltaic industry development, being that electricity conversion is low on the one hand, is high expensive on the other hand.Photovoltaic silicon wafer is the basic material producing solar cell and assembly, and the polysilicon purity for the production of photovoltaic silicon wafer must more than 6N level (namely non-silicon content of impurities is at below 1ppm), otherwise the performance of photovoltaic cell will be subject to very large negative impact.In recent years, polysilicon chip production technology has had marked improvement, polycrystalline cast ingot technology from each silicon ingot of G4(heavily about 270 kilograms, can cut 4 × 4=16 silicon side) progressive to G5 (5 × 5=25 silicon side), then progressive to G6 (6 × 6=36 silicon side) again.Further, produce polycrystalline silicon ingot casting unit volume progressively increase, yield rate increases, and the manufacturing cost of unit volume polycrystalline silicon ingot casting progressively reduces.At present, how producing the polycrystalline silicon ingot casting that volume is larger, is the important measures reducing manufacturing cost.
In actual production process, during solar energy polycrystalline silicon ingot casting, quartz crucible need be used to load silicon material, and after silicon material is dropped into quartz crucible, also need under normal circumstances, through preheating, fusing (also claiming melt), the long brilliant step such as (also weighed to solidification and crystallization), annealing, cooling, just can complete polycrystalline silicon ingot casting process.Actual when carrying out polycrystalline silicon ingot casting, the control of long brilliant process directly has influence on quality and the yield rate of ingot casting finished product, if crystal growth is stablized can obtain higher minority carrier life time and good yield rate; If crystal growing process controls bad, sticky crucible may be caused, the defect such as crystalline substance splits, Hard Inclusion, crystallite, directly affect yield rate.And nowadays, when carrying out polycrystalline silicon ingot casting, most of producer all accurately can not control long brilliant process, thus cause sticky crucible, the defect such as crystalline substance splits, Hard Inclusion, crystallite.
Summary of the invention
Technical problem to be solved by this invention is for above-mentioned deficiency of the prior art, a kind of polycrystalline silicon casting ingot process is provided, its method steps is simple, reasonable in design, it is convenient to realize and be easy to grasp, result of use is good, conservative control can be carried out to the long brilliant process of polycrystalline silicon ingot casting, and effectively improve polycrystalline silicon ingot casting quality.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of polycrystalline silicon casting ingot process
A kind of polycrystalline silicon casting ingot process, is characterized in that this technique comprises the following steps:
Step one, preheating: adopt ingot furnace to carry out preheating to the silicon material be loaded in crucible, and the Heating temperature of described ingot furnace is progressively promoted to T1; Warm up time is 6h ~ 10h, wherein T1=1165 DEG C ~ 1185 DEG C;
Step 2, fusing: adopt described ingot furnace to melt the silicon material be loaded in crucible, until the silicon material in crucible all melts; Temperature of fusion is T1 ~ T5; Wherein T5=1540 DEG C ~ 1560 DEG C;
In this step in melting process, in described ingot furnace, be filled with rare gas element and described ingot furnace internal gas pressure is remained on Q1, wherein Q1=550mbar ~ 650mbar;
Step 3, long crystalline substance: after the Heating temperature of described ingot furnace is down to T6 gradually by T5, start to carry out directional freeze and enter long brilliant process, wherein T6 is polysilicon crystal temperature and T6=1420 DEG C ~ 1440 DEG C; Long brilliant process is as follows:
Step 301, by the heating and temperature control of described ingot furnace at T6, and be incubated 50min ~ 70min; In this step, the heat-insulation cage lift height of described ingot furnace is 60mm ~ 100mm;
Step 302, by the heating and temperature control of described ingot furnace at T6, and be incubated 100min ~ 140min; In this step, the heat-insulation cage lift height of described ingot furnace is identical with the lift height in step 301;
Step 303, by the heating and temperature control of described ingot furnace at T6, and be incubated 160min ~ 200min; In this step, the heat-insulation cage lift height of described ingot furnace is 105mm ~ 115mm;
Step 304, the Heating temperature of described ingot furnace is down to T7 gradually by T6, temperature fall time is 7h ~ 9h; In this step, the heat-insulation cage lift height of described ingot furnace is 205mm ~ 215mm; Wherein, T7=1405 DEG C ~ 1425 DEG C;
Step 305, by the heating and temperature control of described ingot furnace at T7, and be incubated 7h ~ 9h; In this step, the heat-insulation cage lift height of described ingot furnace is identical with the lift height in step 304;
Step 306, by the heating and temperature control of described ingot furnace at T7, and be incubated 7h ~ 9h; In this step, the heat-insulation cage lift height of described ingot furnace is identical with the lift height in step 304;
Step 307, the Heating temperature of described ingot furnace is down to T8 gradually by T7, temperature fall time is 4h ~ 5.5h; In this step, the heat-insulation cage lift height of described ingot furnace is identical with the lift height in step 304; Wherein, T8=1395 DEG C ~ 1415 DEG C;
Step 4, annealing and cooling: after in step 3, long brilliant process completes, carry out annealing and cool, and obtaining the polycrystalline silicon ingot casting of machine-shaping.
Above-mentioned a kind of polycrystalline silicon casting ingot process, it is characterized in that: after in step 3, long brilliant process completes, obtain polycrystal silicon ingot, described polycrystal silicon ingot be divided into highly for h1 top segment, be highly the bottom segment of h1 and the intermediate section that is connected between described top segment and described bottom segment; Carry out annealing to described polycrystal silicon ingot in step 4 and cool, and obtaining the polycrystalline silicon ingot casting of machine-shaping; Wherein, h1=30mm ~ 55mm;
In step 3 in long brilliant process, the brilliant speed of the length of described polycrystal silicon ingot is controlled, the top segment of wherein said polycrystal silicon ingot and the brilliant speed of the length of bottom segment all≤10mm/h, the brilliant speed of length of the intermediate section of described polycrystal silicon ingot is 13mm/h ~ 16mm/h.
Above-mentioned a kind of polycrystalline silicon casting ingot process, is characterized in that: T6=1420 DEG C, T7=1405 DEG C in step 3, T8=1395 DEG C; In step 301, soaking time is 1h, and the heat-insulation cage lift height of described ingot furnace is 90mm; In step 302, soaking time is 2h; In step 303, soaking time is 3h, and the heat-insulation cage lift height of described ingot furnace is 110mm; In step 304, temperature fall time is 9h, and the heat-insulation cage lift height of described ingot furnace is 210mm; In step 305 and step 306, soaking time is 9h; In step 307, temperature fall time is 5h.
Above-mentioned a kind of polycrystalline silicon casting ingot process, it is characterized in that: when annealing in step 4, process is as follows:
Step 401, cooling: the Heating temperature of described ingot furnace is down to T9 gradually by T8, and temperature fall time is 50min ~ 70min; Wherein, T9=1370 DEG C ~ 1390 DEG C;
Step 402, insulation: by the heating and temperature control of described ingot furnace at T9, and be incubated 50min ~ 70min;
Step 403, cooling: the Heating temperature of described ingot furnace is down to T10 gradually by T9, and temperature fall time is 2h ~ 3h; Wherein T10=1100 DEG C ~ 1200 DEG C.
Above-mentioned a kind of polycrystalline silicon casting ingot process, is characterized in that: after having annealed in step 403, when cooling, the Heating temperature of described ingot furnace is down to 400 DEG C gradually by T10, and cooling time is 10h ~ 14h.
Above-mentioned a kind of polycrystalline silicon casting ingot process, it is characterized in that: in step 2 after the silicon material in crucible all melts, first by the heating and temperature control of described ingot furnace at T5, the heating power of described ingot furnace starts to decline afterwards, until described ingot furnace heating power stop decline and after time length t, melt process completes; Then enter step 3 then; Wherein t=18min ~ 22min.
Above-mentioned a kind of polycrystalline silicon casting ingot process, it is characterized in that: when melting in step 2, process is as follows:
1st step, insulation: by the heating and temperature control of described ingot furnace at T1, and be incubated 0.4h ~ 0.6h;
2nd step is to the 5th step, intensification and pressurization: by first the Heating temperature of described ingot furnace being promoted to T2 gradually by T1 to rear point of four steps, the heating-up time is 0.4h ~ 0.6h; In described ingot furnace, be filled with rare gas element in temperature-rise period and the air pressure of described ingot furnace is progressively promoted to Q1; Wherein, T2=1190 DEG C ~ 1210 DEG C;
6th step, first time heat up and pressurize: the Heating temperature of described ingot furnace is promoted to T3 gradually by T2 and the heating-up time is 3.5h ~ 4.5h, the internal gas pressure of ingot furnace described in temperature-rise period remains on Q1; Wherein, T3=1440 DEG C ~ 1460 DEG C;
7th step: second time heats up and pressurize: the Heating temperature of described ingot furnace is promoted to T4 gradually by T3 and the heating-up time is 3.5h ~ 4.5h, and the internal gas pressure of ingot furnace described in temperature-rise period remains on Q1; Wherein, T4=1490 DEG C ~ 1510 DEG C;
8th step, third time heat up and pressurize: the Heating temperature of described ingot furnace is promoted to T5 gradually by T4 and the heating-up time is 3.5h ~ 4.5h, the internal gas pressure of ingot furnace described in temperature-rise period remains on Q1; Wherein, T5=1540 DEG C ~ 1560 DEG C;
9th step, insulation: by the heating and temperature control of described ingot furnace at T5, and be incubated 3.5h ~ 4.5h; In insulating process, described ingot furnace internal gas pressure remains on Q1;
10th step, lasting insulation: by the heating and temperature control of described ingot furnace at T5, and be incubated 4h ~ 8h, until the silicon material in crucible all melts; In insulating process, described ingot furnace internal gas pressure remains on Q1.
Above-mentioned a kind of polycrystalline silicon casting ingot process, is characterized in that: ingot furnace described in step one is G5 type ingot furnace.
Above-mentioned a kind of polycrystalline silicon casting ingot process, is characterized in that: before carrying out long crystalline substance in step 3, also need to carry out impurities removal, and impurities removal process is as follows:
11st step, step-down: by the heating and temperature control of described ingot furnace at T5, and the air pressure of described ingot furnace is down to Q2 by Q1, dip time is 8min ~ 12min; Wherein, Q2=350mbar ~ 450mbar;
12nd step, pressurize: by the heating and temperature control of described ingot furnace at T5, and described ingot furnace internal gas pressure is remained on Q2, the dwell time is 10min ~ 60min;
13rd step, boosting: first the air pressure of described ingot furnace is risen to Q1 by Q2, then the Heating temperature of described ingot furnace is down to T6 gradually by T5, wherein T6 is polysilicon crystal temperature and T6=1420 DEG C ~ 1440 DEG C.
Above-mentioned a kind of polycrystalline silicon casting ingot process, is characterized in that: by when first the Heating temperature of described ingot furnace being promoted to T2 gradually by T1 to rear point of four steps in the 2nd step to the 5th step, and each step promotes temperature 5 DEG C ~ 8 DEG C, and each step promotes and all needs 5min ~ 12min; Carry out in first time intensification and pressure maintaining period in 6th step, carry out in second time intensification and pressure maintaining period in the 7th step, carry out in the 8th step carrying out in insulating process in third time intensification and pressure maintaining period neutralization the 9th step, all need to observe the heating power changing conditions of described ingot furnace, and guarantee that the heating power change of described ingot furnace is steady.
The present invention compared with prior art has the following advantages:
1, reasonable in design and treatment process steps is simple, is easy to grasp.
2, input cost low and realize convenient.
3, easy to operate and melting process end point is used to hold accurately, in melting process, after the silicon material in crucible all melts, the Heating temperature controlling ingot furnace remains unchanged, and observes the time dependent curve of the heating power of ingot furnace (i.e. powertrace); Wherein, after the silicon material in crucible all melts, the powertrace of ingot furnace starts to decline, and to decline and after walking flat 20min, melt process completes, carry out afterwards growing the brilliant stage until the powertrace of ingot furnace.In actual mechanical process, just accurately can determine the time point that melt process completes by observed power curve, be namely switched to some switching time in long brilliant stage by the fusion stage.Actually operating is easy, and realizes conveniently, and energy accurate assurance is switched to the switching time in long brilliant stage by the fusion stage.That is, the present invention stablizes ingot casting melt curve by extending the melt time, the brilliant stage of incision length again after flat 20min is walked until powertrace, thus accurately can be melted to the switching time in long brilliant stage, stop the problem such as polycrystalline silicon ingot casting Quality Down, cost increase because melt deficiency of time or melt overlong time cause simultaneously.Further, employing the present invention can guarantee the quality of long crystalline substance and finally make the efficiency of conversion of cell piece after carrying out accurate assurance to melt in polycrystalline silicon ingot casting process to long brilliant switching time.
4, melting process divides ten steps to carry out, reasonable in design, realize convenient and result of use is good, effectively can improve long crystalloid amount, reduce sticky crucible rate, improve the efficiency of conversion of solar battery sheet, effectively can improve yield rate.
5, sundries discharging method is simple, reasonable in design and impurities removal is effective, reduces stove internal gas pressure rapidly in the 11st step, and reduces air pressure fast and contribute to discharging fast foreign gas, suppresses contact and the absorption of carbonaceous gas and melted silicon; Contribute to the fusing promoting silicon liquid further simultaneously.Further, after rapidly reducing stove internal gas pressure, make carbon-containing impurities in gas no longer at body of heater internal recycle, enhance the convection current of melt and bath surface, make its abundant impurities removal in the 12nd step in pressurize 10 ~ 60min process in the 11st step, impurity discharges body of heater along with air-flow.Thus, by the impurities removal operation in step 3 of the present invention, effectively can reduce the inner impurity of furnace chamber, be easy to obtain more high-purity environment of crystal growth in the long brilliant stage, thus the yield rate of silicon ingot and the overall transformation efficiency of solar battery sheet can effectively be improved, this sundries discharging method is easy to operate, practical, is convenient to batch production.Thus, impurities removal technique of the present invention effectively can reduce the carbon content in silicon ingot process of growth (i.e. long brilliant stage), thus make the silicon ingot of growth have higher quality, and effectively can reduce the generation of Hard Inclusion thus improve silicon ingot yield rate, and reduce wire breaking during cutting of silicon wafers rate, improve solar battery sheet yield rate and efficiency of conversion, this sundries discharging method is easy to operate, practical, is convenient to batch production.
6, grow brilliant process control simple, realize convenient and result of use is good, not only simplify the step of the long brilliant technique of polycrystalline silicon ingot casting, the brilliant temperature course of whole length is allowed more to tend towards stability state, and the object of saving the energy can be reached, effectively can improve long crystalloid amount, reduce sticky crucible rate, improve the efficiency of conversion of solar battery sheet, the method is easy to operate, practical, is convenient to batch production.Meanwhile, in long brilliant process, conservative control is carried out to long brilliant speed, and after the long brilliant process of conservative control, the quality of long crystalline substance can be guaranteed and make the efficiency of conversion of cell piece.Thus, the brilliant technique of length of the present invention stabilizes silicon ingot process of growth more, for long brilliant process provides good environment, avoids the microdefect caused in long brilliant process, enhances practicality, be convenient to batch production.
In sum, the inventive method step is simple, reasonable in design, it is convenient to realize and be easy to grasp, result of use is good, conservative control can be carried out to the long brilliant process of polycrystalline silicon ingot casting, and effectively improve polycrystalline silicon ingot casting quality.
Below by drawings and Examples, technical scheme of the present invention is described in further detail.
Accompanying drawing explanation
Fig. 1 is process flow diagram of the present invention.
Fig. 2 is temperature when adopting the present invention to carry out polycrystalline silicon ingot casting and power.
Embodiment
Embodiment 1
A kind of polycrystalline silicon casting ingot process as shown in Figure 1, comprises the following steps:
Step one, preheating: adopt ingot furnace to carry out preheating to the silicon material be loaded in crucible, and the Heating temperature of described ingot furnace is progressively promoted to T1; Warm up time is 7h, wherein T1=1175 DEG C.
In the present embodiment, described ingot furnace is G5 type ingot furnace.Further, described ingot furnace is specially the G5 type ingot furnace that Zhejiang Jingsheng Electrical and Mechanical Co., Ltd. produces.Described crucible is quartz crucible and it is G5 crucible, and the polycrystalline silicon ingot casting produced is G5 ingot.
During actual use, the charge amount of described quartz crucible is about 600kg.
In the present embodiment, the charge amount of described quartz crucible is 560kg.In actual use procedure, can according to specific needs, the charge amount of described quartz crucible be adjusted accordingly.
In the present embodiment, in step one in warm, the heating power of described ingot furnace is progressively increased to P1, wherein P1=75kW.
Further, in warm, the heating power of described ingot furnace is progressively promoted to P1 with the rate of rise of (10 ~ 15) kW/h.
Actual when carrying out preheating, can according to specific needs, the rate of rise of heating power in warm up time, warm and the value size of T1 and P1 be adjusted accordingly.
Step 2, fusing: adopt described ingot furnace to melt the silicon material be loaded in crucible, temperature of fusion is T1 ~ T5; Wherein T5=1550 DEG C.
In this step in melting process, in described ingot furnace, be filled with rare gas element and described ingot furnace internal gas pressure is remained on Q1, wherein Q1=600mbar.In the present embodiment, described rare gas element is argon gas.
In the present embodiment, after the silicon material in crucible all melts, by the heating and temperature control of described ingot furnace at T5, afterwards the heating power of described ingot furnace start decline, until described ingot furnace heating power stop decline and after time length t, melt process completes; Wherein t=20min.
Actual when melting, can according to specific needs, the value size of T5, t and Q1 be adjusted accordingly.
Step 3, long crystalline substance: after the Heating temperature of described ingot furnace is down to T6 gradually by T5, start to carry out directional freeze and enter long brilliant process, wherein T6 is polysilicon crystal temperature and T6=1420 DEG C; Long brilliant process is as follows:
Step 301, by the heating and temperature control of described ingot furnace at T6, and be incubated 1h; In this step, the heat-insulation cage lift height of described ingot furnace is 90mm.
Herein, heat-insulation cage lift height refers to the height that heat-insulation cage promotes from the warming plate that it is placed, the height namely bottom heat-insulation cage and between warming plate.
Step 302, by the heating and temperature control of described ingot furnace at T6, and be incubated 2h; In this step, the heat-insulation cage lift height of described ingot furnace is identical with the lift height in step 301.
Step 303, by the heating and temperature control of described ingot furnace at T6, and be incubated 3h; In this step, the heat-insulation cage lift height of described ingot furnace is 110mm.
Step 304, the Heating temperature of described ingot furnace is down to T7 gradually by T6, temperature fall time is 9h; In this step, the heat-insulation cage lift height of described ingot furnace is 210mm; Wherein, T7=1405 DEG C.
Step 305, by the heating and temperature control of described ingot furnace at T7, and be incubated 9h; In this step, the heat-insulation cage lift height of described ingot furnace is identical with the lift height in step 304;
Step 306, by the heating and temperature control of described ingot furnace at T7, and be incubated 9h; In this step, the heat-insulation cage lift height of described ingot furnace is identical with the lift height in step 304;
Step 307, the Heating temperature of described ingot furnace is down to T8 gradually by T7, temperature fall time is 5h; In this step, the heat-insulation cage lift height of described ingot furnace is identical with the lift height in step 304; Wherein, T8=1395 DEG C.
Step 4, annealing and cooling: after in step 3, long brilliant process completes, carry out annealing and cool, and obtaining the polycrystalline silicon ingot casting of machine-shaping.
In the present embodiment, when annealing in step 4, process is as follows:
Step 401, cooling: the Heating temperature of described ingot furnace is down to T9 gradually by T8, and temperature fall time is 1h; Wherein, T9=1370 DEG C;
Step 402, insulation: by the heating and temperature control of described ingot furnace at T9, and be incubated 1h;
Step 403, cooling: the Heating temperature of described ingot furnace is down to T10 gradually by T9, and temperature fall time is 2h ~ 3h; Wherein T10=1100 DEG C ~ 1200 DEG C.
In the present embodiment, in step 4, total time needed for annealing process is 4h ~ 5h.
In the present embodiment, after having annealed in step 403, when cooling, the Heating temperature of described ingot furnace is down to 400 DEG C gradually by T10, and cooling time is 10h ~ 14h.
In the present embodiment, when annealing in step 4, the heat-insulation cage of described ingot furnace does not promote, and namely described heat-insulation cage is positioned on warming plate.Carry out in step 4 annealing and in process of cooling, described ingot furnace internal gas pressure being remained on Q1.
In the present embodiment, after long brilliant process completes in step 3, obtain polycrystal silicon ingot, described polycrystal silicon ingot be divided into highly for h1 top segment, be highly the bottom segment of h1 and the intermediate section that is connected between described top segment and described bottom segment; Carry out annealing to described polycrystal silicon ingot in step 4 and cool, and obtaining the polycrystalline silicon ingot casting of machine-shaping.
Meanwhile, actually carry out growing in brilliant process, the long brilliant curve of ingot casting need be stablized by measuring the long brilliant time, guaranteeing the long brilliant speed of ingot casting.In the present embodiment, in step 3 in long brilliant process, the brilliant speed of the length of described polycrystal silicon ingot is controlled, the top segment of wherein said polycrystal silicon ingot and the brilliant speed of the length of bottom segment all≤10mm/h, the brilliant speed of length of the intermediate section of described polycrystal silicon ingot is 13mm/h ~ 16mm/h.In the present embodiment, h1=50mm.
In the present embodiment, before carrying out long crystalline substance in step 3, also need to carry out impurities removal, and impurities removal process is as follows:
11st step, step-down: by the heating and temperature control of described ingot furnace at T5, and the air pressure of described ingot furnace is down to Q2 by Q1, dip time is 10min; Wherein, Q2=400mbar.
12nd step, pressurize: by the heating and temperature control of described ingot furnace at T5, and described ingot furnace internal gas pressure is remained on Q2, the dwell time is 30min.
13rd step, boosting and cooling: first the air pressure of described ingot furnace is risen to Q1 by Q2, then the Heating temperature of described ingot furnace is down to T6 gradually by T5, wherein T6 is polysilicon crystal temperature and T6=1420 DEG C ~ 1440 DEG C.
In the present embodiment, after cooling terminates in the 13rd step, directly enter step 301.That is, impurities removal process can see as the long brilliant stage one early stage operation.
In the present embodiment, the pressure rising time in the 13rd step, the air pressure of described ingot furnace being risen to Q1 by Q2 is 8min ~ 12min, and the temperature fall time that the Heating temperature of described ingot furnace is down to T6 gradually by T5 is 1h ~ 2h.
Actual when carrying out impurities removal, can according to specific needs, the value size of dip time, dwell time, pressure rising time and temperature fall time and Q2 be adjusted accordingly.
In the present embodiment, total time needed for impurities removal process is 2.5h.
When 11st step carries out step-down, carry out step-down by the flow reducing described rare gas element; When 13rd step is boosted, boosted by the flow increasing described rare gas element.
Rapidly reduce stove internal gas pressure in 11st step, and reduce air pressure fast and contribute to discharging fast foreign gas, suppress contact and the absorption of carbonaceous gas and melted silicon; Contribute to the fusing promoting silicon liquid further simultaneously.Further, after rapidly reducing stove internal gas pressure, make carbon-containing impurities in gas no longer at body of heater internal recycle, enhance the convection current of melt and bath surface, make its abundant impurities removal in the 12nd step in pressurize 30min process in the 11st step, impurity discharges body of heater along with air-flow.Thus, by the impurities removal operation in step 3 of the present invention, effectively can reduce the inner impurity of furnace chamber, be easy to obtain more high-purity environment of crystal growth in the long brilliant stage, thus the yield rate of silicon ingot and the overall transformation efficiency of solar battery sheet can effectively be improved, this sundries discharging method is easy to operate, practical, is convenient to batch production.
In the present embodiment, in step 2 after the silicon material in crucible all melts, by the heating and temperature control of described ingot furnace at T5, and the time dependent curve of the heating power of described ingot furnace (i.e. powertrace) is observed, refer to Fig. 2.In Fig. 2, fine line is the time dependent curve of heating power of described ingot furnace, needs solid line to be the time dependent curve of Heating temperature of described ingot furnace, and vertical line is the alarming line of the silicon material in crucible when all melting.As seen from Figure 2, after the silicon material in crucible all melts, the powertrace of described ingot furnace starts to decline, until described ingot furnace powertrace decline and after walking flat 20min, melt process completes, enter the impurities removal stage afterwards, until the impurities removal stage proportionately after, then enter long brilliant; Namely the time point that the A point in Fig. 2 completes for melt process.
In actual mechanical process, just the time point that melt process completes accurately can be determined by observed power curve, namely the impurities removal stage is switched to (wherein by the fusion stage, the impurities removal stage also can regard the operation in early stage in long brilliant stage as) some switching time, the impurities removal stage is switched to by the fusion stage by energy accurate assurance of the present invention, and actual to the switching in long brilliant stage from the impurities removal stage, actually operating is easy, and realizes conveniently.That is, the end time point of melt process accurately can be grasped by the present invention, with solve cause because of melt deficiency of time or melt overlong time the problem of production polycrystalline silicon ingot casting Quality Down, wherein during melt deficiency of time, silicon material may be caused to melt abundant not, cause the silicon ingot life-span abnormal; And if melt overlong time, quartz crucible will be made to be in hot stage for a long time, damage may to be caused to silicon nitride coating, cause sticky crucible.
In the present embodiment, after the silicon material in crucible described in step 2 all melts, the heating power changing conditions of described ingot furnace is observed, treat that the heating power of described ingot furnace drops to P2, and keep P2 constant and after time length t, melt process completes; Wherein, P2=40kW.
Actual when melting, according to the difference of charge amount in described crucible, the size of P2 is corresponding to be adjusted within the scope of 35kW ~ 45kW.
In the present embodiment, when melting in step 2, process is as follows:
1st step, insulation: by the heating and temperature control of described ingot furnace at T1, and be incubated 0.5h.
2nd step is to the 5th step, intensification and pressurization: by first the Heating temperature of described ingot furnace being promoted to T2 gradually by T1 to rear point of four steps, the heating-up time be 0.5h(i.e. the 2nd step to total time of the 5th step be 0.5h); In described ingot furnace, be filled with rare gas element in temperature-rise period and the air pressure of described ingot furnace is progressively promoted to Q1; Wherein, T2=1200 DEG C.
By when first the Heating temperature of described ingot furnace being promoted to T2 gradually by T1 to rear point of four steps in 2nd step to the 5th step, each step promotes temperature 5 DEG C ~ 8 DEG C, and each step promotes and all needs 5min ~ 10min.
6th step, first time heat up and pressurize: the Heating temperature of described ingot furnace is promoted to T3 gradually by T2 and the heating-up time is 4h, the internal gas pressure of ingot furnace described in temperature-rise period remains on Q1; Wherein, T3=1450 DEG C.
7th step: second time heats up and pressurize: the Heating temperature of described ingot furnace is promoted to T4 gradually by T3 and the heating-up time is 4h, and the internal gas pressure of ingot furnace described in temperature-rise period remains on Q1; Wherein, T4=1500 DEG C.
8th step, third time heat up and pressurize: the Heating temperature of described ingot furnace is promoted to T5 gradually by T4 and the heating-up time is 4h, the internal gas pressure of ingot furnace described in temperature-rise period remains on Q1; Wherein, T5=1550 DEG C.
9th step, insulation: by the heating and temperature control of described ingot furnace at T5, and be incubated 4h; In insulating process, described ingot furnace internal gas pressure remains on Q1.
10th step, lasting insulation: by the heating and temperature control of described ingot furnace at T5, and be incubated 6h, until the silicon material in crucible all melts; In insulating process, described ingot furnace internal gas pressure remains on Q1.
In the present embodiment, carry out in first time intensification and pressure maintaining period in 6th step, carry out in second time intensification and pressure maintaining period in the 7th step, carry out in the 8th step carrying out in insulating process in third time intensification and pressure maintaining period neutralization the 9th step, all need to observe the heating power changing conditions of described ingot furnace, and guarantee that the heating power change of described ingot furnace is steady.
That is, when melting in the 6th step to the 9th step, powertrace must be made steadily to advance, comparatively significantly sags and crests can not be occurred, increasing of Hard Inclusion can be brought like this.
In the present embodiment, when carrying out heating up and pressurizeing in the 2nd step to the 5th step, process is as follows:
2nd step, the first step promote: the Heating temperature of described ingot furnace is promoted to 1182 DEG C by 1175 DEG C, and the heating-up time is 7min.
3rd step, second step promote: the Heating temperature of described ingot furnace is promoted to 1190 DEG C by 1182 DEG C, and the heating-up time is 8min.
4th step, the 3rd step promote: the Heating temperature of described ingot furnace is promoted to 1195 DEG C by 1190 DEG C, and the heating-up time is 5min.
5th step, the 4th step promote: the Heating temperature of described ingot furnace is promoted to 1200 DEG C by 1195 DEG C, and the heating-up time is 5min.
In the present embodiment, in 10th step after the silicon material in crucible all melts and described ingot furnace sends " fusing completes warning ", need manual intervention, the decline situation of powertrace is observed, until described ingot furnace powertrace decline and after walking flat 20min, melt process completes, and manual intervention afterwards will be cut into the long brilliant stage fusion stage.
In the present embodiment, process any surface finish, the inclusion-free of forming polycrystalline silicon ingot casting, without sticky crucible phenomenon, minority carrier life time >5.5us (microsecond), Hard Inclusion ratio <0.5%, yield rate is 70.5%.Use institute process forming polycrystalline silicon ingot casting to make silicon chip and to cut into slices afterwards stria ratio <0.5%, solar battery sheet efficiency of conversion can improve 0.1%.
Embodiment 2
In the present embodiment, as different from Example 1: in step one, warm up time is 6h and T1=1185 DEG C, P1=80kW; T5=1560 DEG C, t=18min, Q1=650mbar in step 2; In 1st step, soaking time is 0.4h; T2=1210 DEG C in 2nd step to the 5th step, the heating-up time is 0.4h; In 6th step, T3=1460 DEG C and heating-up time are 3.5h; In 7th step, T4=1510 DEG C and heating-up time are 3.5h; In 8th step, T5=1560 DEG C and heating-up time are 3.5h; In 9th step, soaking time is 3.5h; In 10th step, soaking time is 4h.
In the present embodiment, when carrying out heating up and pressurizeing in the 2nd step to the 5th step, process is as follows:
2nd step, the first step promote: the Heating temperature of described ingot furnace is promoted to 1190 DEG C by 1185 DEG C, and the heating-up time is 5min.
3rd step, second step promote: the Heating temperature of described ingot furnace is promoted to 1195 DEG C by 1190 DEG C, and the heating-up time is 5min.
4th step, the 3rd step promote: the Heating temperature of described ingot furnace is promoted to 1205 DEG C by 1195 DEG C, and the heating-up time is 9min.
5th step, the 4th step promote: the Heating temperature of described ingot furnace is promoted to 1210 DEG C by 1205 DEG C, and the heating-up time is 5min.
In the present embodiment, when carrying out impurities removal, in the 11st step, dip time is 8min and Q2=450mbar; In 12nd step, the dwell time is 60min; In 13rd step, pressure rising time is 8min.Further, total time needed for impurities removal process is 2.6h.
In the present embodiment, when carrying out long crystalline substance in step 3, in step 301, soaking time is 50min and heat-insulation cage lift height is 85mm; In step 302, soaking time is 100min; Step 303 soaking time is 160min and heat-insulation cage lift height is 105mm; In step 304, temperature fall time is 7h and T7=1425 DEG C; In step 305 and step 306, soaking time is 7h; In step 307, soaking time is 4h and T8=1415 DEG C; H1=45mm.
In the present embodiment, when annealing in step 4, in step 401, temperature fall time is 50min and T9=1390 DEG C; In step 402, soaking time is 50min.
In the present embodiment, all the other processing steps and processing parameter are all identical with embodiment 1.
In the present embodiment, process any surface finish, the inclusion-free of forming polycrystalline silicon ingot casting, without sticky crucible phenomenon, minority carrier life time >5.7us (microsecond), Hard Inclusion ratio <0.5%, yield rate is 71%.Use institute process forming polycrystalline silicon ingot casting to make silicon chip and to cut into slices afterwards stria ratio <0.5%, solar battery sheet efficiency of conversion can improve 0.1%.
Embodiment 3
In the present embodiment, as different from Example 1: in step one, warm up time is 10h and T1=1165 DEG C, P1=70kW; T5=1540 DEG C, t=22min, Q1=550mbar in step 2; In 1st step, soaking time is 0.6h; T2=1190 DEG C in 2nd step to the 5th step, the heating-up time is 0.6h; In 6th step, T3=1440 DEG C and heating-up time are 4.5h; In 7th step, T4=1490 DEG C and heating-up time are 4.5h; In 8th step, T5=1540 DEG C and heating-up time are 4.5h; In 9th step, soaking time is 4.5h; In 10th step, soaking time is 8h.
In the present embodiment, when carrying out heating up and pressurizeing in the 2nd step to the 5th step, process is as follows:
2nd step, the first step promote: the Heating temperature of described ingot furnace is promoted to 1172 DEG C by 1165 DEG C, and the heating-up time is 9min.
3rd step, second step promote: the Heating temperature of described ingot furnace is promoted to 1178 DEG C by 1172 DEG C, and the heating-up time is 8min.
4th step, the 3rd step promote: the Heating temperature of described ingot furnace is promoted to 1183 DEG C by 1178 DEG C, and the heating-up time is 10min.
5th step, the 4th step promote: the Heating temperature of described ingot furnace is promoted to 1190 DEG C by 1183 DEG C, and the heating-up time is 9min.
In the present embodiment, when carrying out impurities removal, in the 11st step, dip time is 12min and Q2=350mbar; In 12nd step, the dwell time is 35min; In 13rd step, pressure rising time is 12min.
In the present embodiment, total time needed for impurities removal process is 2.4h.
In the present embodiment, when carrying out long crystalline substance in step 3, in step 301, soaking time is 70min and heat-insulation cage lift height is 95mm; In step 302, soaking time is 140min; Step 303 soaking time is 200min and heat-insulation cage lift height is 115mm; In step 304, temperature fall time is 8h and T7=1415 DEG C; In step 305 and step 306, soaking time is 7h; In step 307, soaking time is 5.5h and T8=1405 DEG C; H1=55mm.
In the present embodiment, when annealing in step 4, in step 401, temperature fall time is 70min and T9=1380 DEG C; In step 402, soaking time is 70min.
In the present embodiment, all the other processing steps and processing parameter are all identical with embodiment 1.
In the present embodiment, process any surface finish, the inclusion-free of forming polycrystalline silicon ingot casting, without sticky crucible phenomenon, minority carrier life time >5.0us (microsecond), Hard Inclusion ratio <0.5%, yield rate is 70%.Use institute process forming polycrystalline silicon ingot casting to make silicon chip and to cut into slices afterwards stria ratio <0.5%, solar battery sheet efficiency of conversion can improve 0.1%.
Embodiment 4
In the present embodiment, as different from Example 1: when carrying out impurities removal, in the 11st step, dip time is 10min and Q2=380mbar; In 12nd step, the dwell time is 25min; In 13rd step, pressure rising time is 10min; H1=40mm.
In the present embodiment, total time needed for impurities removal process is 2.5h.
In the present embodiment, when carrying out long crystalline substance in step 3, in step 301, soaking time is 70min and heat-insulation cage lift height is 60mm.
In the present embodiment, all the other processing steps and processing parameter are all identical with embodiment 1.
In the present embodiment, process any surface finish, the inclusion-free of forming polycrystalline silicon ingot casting, without sticky crucible phenomenon, minority carrier life time >5.0us (microsecond), Hard Inclusion ratio <0.5%, yield rate is 70%.Use institute process forming polycrystalline silicon ingot casting to make silicon chip and to cut into slices afterwards stria ratio <0.5%, solar battery sheet efficiency of conversion can improve 0.1%.
Embodiment 5
In the present embodiment, as different from Example 1: when carrying out impurities removal, in the 11st step, dip time is 10min and Q2=450mbar; In 12nd step, the dwell time is 10min; In 13rd step, pressure rising time is 10min; H1=30mm.
In the present embodiment, total time needed for impurities removal process is 2.5h.
In the present embodiment, when carrying out long crystalline substance in step 3, in step 301, soaking time is 70min and heat-insulation cage lift height is 100mm.
In the present embodiment, all the other processing steps and processing parameter are all identical with embodiment 1.
In the present embodiment, process any surface finish, the inclusion-free of forming polycrystalline silicon ingot casting, without sticky crucible phenomenon, minority carrier life time >5.0us (microsecond), Hard Inclusion ratio <0.5%, yield rate is 70%.Use institute process forming polycrystalline silicon ingot casting to make silicon chip and to cut into slices afterwards stria ratio <0.5%, solar battery sheet efficiency of conversion can improve 0.05%.
The above; it is only preferred embodiment of the present invention; not the present invention is imposed any restrictions, every above embodiment is done according to the technology of the present invention essence any simple modification, change and equivalent structure change, all still belong in the protection domain of technical solution of the present invention.
Claims (10)
1. a polycrystalline silicon casting ingot process, is characterized in that this technique comprises the following steps:
Step one, preheating: adopt ingot furnace to carry out preheating to the silicon material be loaded in crucible, and the Heating temperature of described ingot furnace is progressively promoted to T1; Warm up time is 6h ~ 10h, wherein T1=1165 DEG C ~ 1185 DEG C;
Step 2, fusing: adopt described ingot furnace to melt the silicon material be loaded in crucible, until the silicon material in crucible all melts; Temperature of fusion is T1 ~ T5; Wherein T5=1540 DEG C ~ 1560 DEG C;
In this step in melting process, in described ingot furnace, be filled with rare gas element and described ingot furnace internal gas pressure is remained on Q1, wherein Q1=550mbar ~ 650mbar;
Step 3, long crystalline substance: after the Heating temperature of described ingot furnace is down to T6 gradually by T5, start to carry out directional freeze and enter long brilliant process, wherein T6 is polysilicon crystal temperature and T6=1420 DEG C ~ 1440 DEG C; Long brilliant process is as follows:
Step 301, by the heating and temperature control of described ingot furnace at T6, and be incubated 50min ~ 70min; In this step, the heat-insulation cage lift height of described ingot furnace is 60mm ~ 100mm;
Step 302, by the heating and temperature control of described ingot furnace at T6, and be incubated 100min ~ 140min; In this step, the heat-insulation cage lift height of described ingot furnace is identical with the lift height in step 301;
Step 303, by the heating and temperature control of described ingot furnace at T6, and be incubated 160min ~ 200min; In this step, the heat-insulation cage lift height of described ingot furnace is 105mm ~ 115mm;
Step 304, the Heating temperature of described ingot furnace is down to T7 gradually by T6, temperature fall time is 7h ~ 9h; In this step, the heat-insulation cage lift height of described ingot furnace is 205mm ~ 215mm; Wherein, T7=1405 DEG C ~ 1425 DEG C;
Step 305, by the heating and temperature control of described ingot furnace at T7, and be incubated 7h ~ 9h; In this step, the heat-insulation cage lift height of described ingot furnace is identical with the lift height in step 304;
Step 306, by the heating and temperature control of described ingot furnace at T7, and be incubated 7h ~ 9h; In this step, the heat-insulation cage lift height of described ingot furnace is identical with the lift height in step 304;
Step 307, the Heating temperature of described ingot furnace is down to T8 gradually by T7, temperature fall time is 4h ~ 5.5h; In this step, the heat-insulation cage lift height of described ingot furnace is identical with the lift height in step 304; Wherein, T8=1395 DEG C ~ 1415 DEG C;
Step 4, annealing and cooling: after in step 3, long brilliant process completes, carry out annealing and cool, and obtaining the polycrystalline silicon ingot casting of machine-shaping.
2. according to a kind of polycrystalline silicon casting ingot process according to claim 1, it is characterized in that: after in step 3, long brilliant process completes, obtain polycrystal silicon ingot, described polycrystal silicon ingot be divided into highly for h1 top segment, be highly the bottom segment of h1 and the intermediate section that is connected between described top segment and described bottom segment; Carry out annealing to described polycrystal silicon ingot in step 4 and cool, and obtaining the polycrystalline silicon ingot casting of machine-shaping; Wherein, h1=30mm ~ 55mm;
In step 3 in long brilliant process, the brilliant speed of the length of described polycrystal silicon ingot is controlled, the top segment of wherein said polycrystal silicon ingot and the brilliant speed of the length of bottom segment all≤10mm/h, the brilliant speed of length of the intermediate section of described polycrystal silicon ingot is 13mm/h ~ 16mm/h.
3. according to a kind of polycrystalline silicon casting ingot process described in claim 1 or 2, it is characterized in that: T6=1420 DEG C, T7=1405 DEG C in step 3, T8=1395 DEG C; In step 301, soaking time is 1h, and the heat-insulation cage lift height of described ingot furnace is 90mm; In step 302, soaking time is 2h; In step 303, soaking time is 3h, and the heat-insulation cage lift height of described ingot furnace is 110mm; In step 304, temperature fall time is 9h, and the heat-insulation cage lift height of described ingot furnace is 210mm; In step 305 and step 306, soaking time is 9h; In step 307, temperature fall time is 5h.
4., according to a kind of polycrystalline silicon casting ingot process described in claim 1 or 2, it is characterized in that: when annealing in step 4, process is as follows:
Step 401, cooling: the Heating temperature of described ingot furnace is down to T9 gradually by T8, and temperature fall time is 50min ~ 70min; Wherein, T9=1370 DEG C ~ 1390 DEG C;
Step 402, insulation: by the heating and temperature control of described ingot furnace at T9, and be incubated 50min ~ 70min;
Step 403, cooling: the Heating temperature of described ingot furnace is down to T10 gradually by T9, and temperature fall time is 2h ~ 3h; Wherein T10=1100 DEG C ~ 1200 DEG C.
5. according to a kind of polycrystalline silicon casting ingot process according to claim 4, it is characterized in that: after having annealed in step 403, when cooling, the Heating temperature of described ingot furnace is down to 400 DEG C gradually by T10, and cooling time is 10h ~ 14h.
6. according to a kind of polycrystalline silicon casting ingot process described in claim 1 or 2, it is characterized in that: in step 2 after the silicon material in crucible all melts, first by the heating and temperature control of described ingot furnace at T5, the heating power of described ingot furnace starts to decline afterwards, until described ingot furnace heating power stop decline and after time length t, melt process completes; Then enter step 3 then; Wherein t=18min ~ 22min.
7., according to a kind of polycrystalline silicon casting ingot process described in claim 1 or 2, it is characterized in that: when melting in step 2, process is as follows:
1st step, insulation: by the heating and temperature control of described ingot furnace at T1, and be incubated 0.4h ~ 0.6h;
2nd step is to the 5th step, intensification and pressurization: by first the Heating temperature of described ingot furnace being promoted to T2 gradually by T1 to rear point of four steps, the heating-up time is 0.4h ~ 0.6h; In described ingot furnace, be filled with rare gas element in temperature-rise period and the air pressure of described ingot furnace is progressively promoted to Q1; Wherein, T2=1190 DEG C ~ 1210 DEG C;
6th step, first time heat up and pressurize: the Heating temperature of described ingot furnace is promoted to T3 gradually by T2 and the heating-up time is 3.5h ~ 4.5h, the internal gas pressure of ingot furnace described in temperature-rise period remains on Q1; Wherein, T3=1440 DEG C ~ 1460 DEG C;
7th step: second time heats up and pressurize: the Heating temperature of described ingot furnace is promoted to T4 gradually by T3 and the heating-up time is 3.5h ~ 4.5h, and the internal gas pressure of ingot furnace described in temperature-rise period remains on Q1; Wherein, T4=1490 DEG C ~ 1510 DEG C;
8th step, third time heat up and pressurize: the Heating temperature of described ingot furnace is promoted to T5 gradually by T4 and the heating-up time is 3.5h ~ 4.5h, the internal gas pressure of ingot furnace described in temperature-rise period remains on Q1; Wherein, T5=1540 DEG C ~ 1560 DEG C;
9th step, insulation: by the heating and temperature control of described ingot furnace at T5, and be incubated 3.5h ~ 4.5h; In insulating process, described ingot furnace internal gas pressure remains on Q1;
10th step, lasting insulation: by the heating and temperature control of described ingot furnace at T5, and be incubated 4h ~ 8h, until the silicon material in crucible all melts; In insulating process, described ingot furnace internal gas pressure remains on Q1.
8. according to a kind of polycrystalline silicon casting ingot process described in claim 1 or 2, it is characterized in that: ingot furnace described in step one is G5 type ingot furnace.
9. according to a kind of polycrystalline silicon casting ingot process described in claim 1 or 2, it is characterized in that: before carrying out long crystalline substance in step 3, also need to carry out impurities removal, and impurities removal process be as follows:
11st step, step-down: by the heating and temperature control of described ingot furnace at T5, and the air pressure of described ingot furnace is down to Q2 by Q1, dip time is 8min ~ 12min; Wherein, Q2=350mbar ~ 450mbar;
12nd step, pressurize: by the heating and temperature control of described ingot furnace at T5, and described ingot furnace internal gas pressure is remained on Q2, the dwell time is 10min ~ 60min;
13rd step, boosting: first the air pressure of described ingot furnace is risen to Q1 by Q2, then the Heating temperature of described ingot furnace is down to T6 gradually by T5, wherein T6 is polysilicon crystal temperature and T6=1420 DEG C ~ 1440 DEG C.
10. according to a kind of polycrystalline silicon casting ingot process according to claim 7, it is characterized in that: by when first the Heating temperature of described ingot furnace being promoted to T2 gradually by T1 to rear point of four steps in the 2nd step to the 5th step, each step promotes temperature 5 DEG C ~ 8 DEG C, and each step lifting all needs 5min ~ 12min; Carry out in first time intensification and pressure maintaining period in 6th step, carry out in second time intensification and pressure maintaining period in the 7th step, carry out in the 8th step carrying out in insulating process in third time intensification and pressure maintaining period neutralization the 9th step, all need to observe the heating power changing conditions of described ingot furnace, and guarantee that the heating power change of described ingot furnace is steady.
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| CN105220227A (en) * | 2015-10-27 | 2016-01-06 | 天津英利新能源有限公司 | A kind of efficient polycrystalline silicon casting ingot process |
| CN105780109A (en) * | 2016-04-08 | 2016-07-20 | 江西旭阳雷迪高科技股份有限公司 | Device and method for improving edge grain tilting growth of polycrystalline ingot furnace |
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