CN103436955A - Process control method for directional solidification of polycrystalline silicon - Google Patents
Process control method for directional solidification of polycrystalline silicon Download PDFInfo
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Abstract
The invention belongs to the field of directional solidification, and particularly relates to a process control method for directional solidification of polycrystalline silicon, wherein temperatures of an upper portion heating device, a middle portion heating device and a lower portion heating device are separately adjusted after a silicon material is melted to carry out crystal growth and annealing cooling on the silicon body, and finally the ingot is taken. With the present invention, a furnace space can be maximally utilized, and an equipment investment cost can be saved; and the temperatures of the lower portion heating device and the middle portion heating device are controlled, and the water cooling manner is adopted to reduce the temperature of the bottom of the crucible so as to rapid cool, such that energy consumption per unit mass of the casting ingot is reduced.
Description
Technical field
The invention belongs to the directional freeze field, particularly a kind of process control method of polysilicon directional freezing.
Background technology
Directional freeze refers to and adopt compulsive means in process of setting, sets up the thermograde of specific direction in the melt of He Wei frozen metal, frozen metal, thereby melt is solidified along the direction contrary with hot-fluid, finally obtains having the technology of specific orientation column crystal.Directional freeze is the important means of research solidification theory and metal freezing rule, is also the important method for preparing monocrystal material and the brilliant high performance structures material of micron order (or nano level) continuous fibre and functional materials.Since the sixties in 20th century, the directional solidification technique development is very fast.Developed into high speed freezing method, liquid metal method of cooling and the continuous directional solidification technology of current widespread use by initial heat-generating agent method, power reduction method.Directional solidification technique is widely used in the power faces such as preparation of superalloy, magneticsubstance, single crystal growing, in-situ composite, and compound, shape memory alloy field have extremely wide application prospect between the class single-crystal metal.
Existing polycrystalline silicon ingot or purifying furnace is to adopt resistance or induction heating, after by proportioning, good polysilicon is put into square crucible and is melted, by doing relative motion between the spare part to forming thermal field, so that polycrystalline silicon material begins to cool down from bottom, the mode of long brilliant directional freeze upwards gradually, obtain polycrystal silicon ingot.Estimate an energy consumption that important indicator is unit mass of polycrystalline silicon ingot or purifying furnace performance, and reduce the energy consumption of unit mass, and then to reduce costs be the win the market important means of competition of enterprise.The major way of the energy consumption of enterprise's reduction in the market is to improve single stove production capacity, from single furnace output 120kg of 2004, and to 170kg, 250kg, 450kg, 650kg.
At present, the production capacity of main flow polycrystalline silicon ingot or purifying furnace maximum is 660 kilograms on the market.Be accompanied by the increase of single stove production capacity, the inevitable corresponding increasing of single silicon ingot size, and in the long brilliant stage of ingot casting, the silicon ingot bottom is first cooling, cooling behind top, crystal could slowly be grown from bottom to top like this, and the cooling of top constantly taken heat to bottom and carry out by the bottom silicon crystal.And if silicon ingot is oversize, so, due to the thermal conductivity of silicon crystal bad, therefore the temperature difference at bottom and top will be excessive and generation stress, in addition, the long meeting of crystal causes being out of shape in crystal growing process, and, the more important thing is, excessive silicon ingot brings difficulty to the manufacture of crucible and the processing of silicon ingot and the evolution of silicon ingot, not only need novel support equipment, and, bring very large challenge to the cost of the auxiliaries such as crucible of these support equipments.Therefore, improve merely single stove production capacity and faced bottleneck with the method that reduces the unit mass energy consumption.
Summary of the invention
The present invention overcomes above-mentioned not enough problem, and a kind of process control method of polysilicon directional freezing is provided, and can utilize to greatest extent furnace space, saves equipment investment cost.Simultaneously, the temperature by controlling bottom heating unit and middle part heating unit and the mode of water-cooled realize the reduction of described crucible bottom temperature, make speed of cooling faster, have therefore reduced the energy consumption of ingot casting unit mass.
The technical scheme that the present invention adopted for achieving the above object is: a kind of process control method of polysilicon directional freezing, first vacuumize, and then in body of heater, pass into argon gas, then, by silicon material heat fused, proceed according to following steps:
(1) progressively reduce the temperature of middle part heating unit and bottom heating unit, and improve the flow velocity of water in rotatable lifting water cold platform mechanism simultaneously, the crucible bottom temperature is reduced gradually, when the crucible bottom temperature during lower than 1414 ℃, crucible bottom starts crystallization and forms polysilicon, when directional freeze during to 45-55%, and then reduce the temperature of top heating unit, make polysilicon continue up growth.
Wherein, the cooling of middle part heating unit and bottom heating unit is carried out according to following preferable procedure: temperature is since 1450 ℃-1500 ℃ declines, initial 3 hours with the per hour speed decline of 15-25 ℃, subsequently with the per hour speed decline of 5-15 ℃, until drop to 950-1000 ℃.
The cooling of top heating unit is preferably carried out according to following program: start to descend from 1460-1500 ℃, with the per hour speed decline of 2-5 ℃, finally be stabilized in 1350-1370 ℃.
In rotatable lifting water cold platform mechanism, the flow velocity of water is preferably 200-300L/min.
(2) anneal cooling: when polysilicon grows into fully, adjust top heating unit, middle part heating unit and bottom heating unit temperature, to the polycrystal silicon ingot rear insulation of being annealed, finally close the power supply of heating unit, allow silicon ingot automatically lower the temperature.
Wherein step (2) is preferably carried out in such a way: after polycrystal silicon ingot grows into fully, improve middle part heating unit and bottom heating unit to 1350-1370 ℃, insulation 1.5-2.5 hour, reduced top heating unit, middle part heating unit and bottom heating unit temperature to 1100-1200 ℃ with 2.5-3.5 hour again, insulation 1.5-2.5 hour; Use again afterwards the temperature that reduces top heating unit, middle part heating unit and bottom heating unit in 2.5-3.5 hour to 800-950 ℃, be incubated 0.5-1.5 hour, finally close the power supply of heating unit, allow silicon ingot automatically lower the temperature.
(3) going out ingot finishes: when the temperature of the polycrystal silicon ingot formed when polysilicon is reduced to below 300 ℃, open bell, start rotatable lifting water cold platform mechanism, crucible is risen to its bottom surface and exceed bell oral thermometer face on body of heater, take out polycrystalline silicon ingot casting, EO.
A kind of polysilicon directional freezing device used in the present invention: comprise body of heater, the upper bell electric screw hoisting appliance external by body of heater that is communicated with vent line is arranged on the body of heater top, lower bell is threaded connection at bottom of furnace body, be mounted with crucible in body of heater, the rotatable lifting water cold platform mechanism be connected with lower bell is fixedly connected with at the bottom of crucible, directly over crucible, the top heating unit is installed in body of heater, it comprises and is arranged on Shang top, furnace wall water-cooled copper electrode, be arranged in addition dependence bolted top Graphite Electrodes and upper portion heater graphite annulus in stove, the sidewall of crucible outside is equipped with the middle part heating unit in body of heater, it comprise the graphite junction station and with the bolted graphite heating rod of its dependence, graphite heating rod one end is connected with the graphite junction station, the other end is connected with fan-shaped graphite splitter, between crucible and lower bell, the bottom heating unit is installed, it comprises and is arranged on the bottom Graphite Electrodes in stove and is fixed in the bottom water-cooled copper electrode on lower bell, and the bottom Graphite Electrodes is fixedly mounted on the water-cooled copper electrode of bottom, the body of heater internal surface is provided with thermal insulation layer, and it comprises the upper insulation cover, the side insulated tank that is positioned at the crucible outer wall that are positioned at directly over crucible, is positioned at lower insulating ring and lower insulation cover under crucible.
The inventive method design is unique, on the basis of existing equipment, innovated improvement, in the situation that thermal field does not relatively move, produce long brilliant required thermograde by the temperature of controlling top heating unit, bottom heating unit and middle part heating unit, form polycrystalline cast ingot.Simple to operate, be easy to control and calculate.
The accompanying drawing explanation
Fig. 1 is a kind of polysilicon directional freezing apparatus structure schematic diagram used in the present invention.
In figure, 1. go up the rotatable lifting water cold platform of 9. times insulation covers of insulation cover 7. side insulated tank 8. bottom insulating rings, the 10. bottom Graphite Electrodes fan-shaped graphite splitter 13. graphite heating rod 14. graphite junction station 15. upper portion heater graphite annulus 16. top Graphite Electrodes 17. top water-cooled copper electrode 18. of 11. bottom water-cooled copper electrode 12. mechanism 19. crucibles on 3. times bells of bell 2. silicon material, 4. electric screw hoisting appliance 5. vent lines 6.
Embodiment
Describe the present invention in detail below in conjunction with specific embodiment and accompanying drawing, but the present invention is not limited to specific embodiment.
Embodiment 1:
A kind of polysilicon directional freezing process control method device used, comprise body of heater, the upper bell 1 electric screw hoisting appliance 4 external by body of heater that is communicated with vent line 5 is arranged on the body of heater top, lower bell 3 is threaded connection at bottom of furnace body, be mounted with crucible 19 in body of heater, the rotatable lifting water cold platform mechanism 18 be connected with lower bell 3 was fixedly connected with 19 ends of crucible, directly over crucible 19, the top heating unit is installed in body of heater, it comprises and is arranged on Shang top, furnace wall water-cooled copper electrode 17, be arranged in addition the bolted top of dependence Graphite Electrodes 16 and upper portion heater graphite annulus 15 in stove, the crucible 19 walls outsides are equipped with the middle part heating unit in body of heater, it comprise graphite junction station 14 and with the bolted graphite heating rod 13 of its dependence, graphite heating rod 13 1 ends are connected with graphite junction station 14, the other end is connected with fan-shaped graphite splitter 12, between crucible 19 and lower bell 3, the bottom heating unit is installed, it comprises the bottom Graphite Electrodes 10 be arranged in stove and is fixed in the bottom water-cooled copper electrode 11 on lower bell 3, and bottom Graphite Electrodes 10 is fixedly mounted on bottom water-cooled copper electrode 11, the body of heater internal surface is provided with thermal insulation layer, and it comprises the upper insulation cover 6, the side insulated tank 7 that is positioned at crucible 19 outer walls that are positioned at directly over crucible 19, is positioned at lower insulating ring 8 and lower insulation cover 9 under crucible 19.
The top heating unit is 100kw, and middle part heating unit and bottom heating unit are 60kw.
Upper portion heater graphite annulus 15 is square structure, and its internal diameter is greater than quartz crucible 19 internal diameters.
The ceramic jacket insulation is installed between top Graphite Electrodes 16 and side insulated tank 7.
The ceramic jacket insulation is installed between top water-cooled copper electrode 17 and body of heater.
Be connected with the Multi-layer graphite carbon paper with the connecting end surface of top Graphite Electrodes 16 at top water-cooled copper electrode 17, in case thermal value is large, cause electrode thread to damage.
The ceramic jacket insulation is installed between bottom Graphite Electrodes 10 and bottom insulating ring 8.
The ceramic jacket insulation is installed between bottom water-cooled copper electrode 11 and lower bell 3.
Bottom water-cooled copper electrode 11 is connected with the Multi-layer graphite carbon paper with the connecting end surface of bottom Graphite Electrodes 10, in case thermal value is large, causes electrode thread to damage.
Embodiment 2:
A kind of process control method of polysilicon directional freezing, adopt device in embodiment 1, and preparation step is as follows:
(1) crucible of the quartzy material of Φ 900mm*600mm 19 is placed in body of heater, and is connected with rotatable lifting water cold platform mechanism 18, the 670kg silicon material of packing into.Crucible 19 is outer surrounds protection with the plumbago crucible backplate.
(2) rotatable lifting water cold platform mechanism 18 drives crucibles 19 and descends, and on closure, bell 1, starts to vacuumize.
(3) when the vacuum tightness of body of heater inside reaches 1Pa, beginning is to applying argon gas in body of heater, when the vacuum tightness of body of heater inside reaches 60000Pa, in startup, heating unit, middle heating unit and lower heating unit, start to heat silicon material 2, through 6 hours, silicon material 2 starts fusing, then continues heating after 4 hours, and the silicon material melts fully, now, be incubated 0.5 hour at the temperature of 1490 ℃.
According to following steps, proceed:
(4) the silicon body is long brilliant: the temperature that progressively reduces middle part heating unit and bottom heating unit, and improve the flow velocity of water in rotatable lifting water cold platform mechanism 18 simultaneously, crucible 19 bottom temps are reduced gradually, when crucible 19 bottom temps during lower than 1414 ℃, crucible 19 bottoms start crystallization and form polysilicon, when directional freeze to 45%, and then the temperature of reduction top heating unit, make polysilicon continue up growth.
The cooling of middle part heating unit and bottom heating unit is carried out according to following program: temperature is since 1450 ℃ of declines, and initial 3 hours with the per hour speed decline of 15 ℃, subsequently with the per hour speed decline of 5 ℃, until drop to 950 ℃.
The cooling of top heating unit is carried out according to following program: since 1460 ℃ of declines, with the per hour speed decline of 2 ℃, finally be stabilized in 1350 ℃.
In rotatable lifting water cold platform mechanism 18, the flow velocity of water is 200L/min.
(5) anneal cooling: when polysilicon grows into fully, adjust top heating unit, middle part heating unit and bottom heating unit temperature, to the polycrystal silicon ingot rear insulation of being annealed, finally close the power supply of heating unit, allow silicon ingot automatically lower the temperature.
Wherein, step (5) is carried out in such a way: after polycrystal silicon ingot grows into fully, improve middle part heating unit and bottom heating unit to 1350 ℃, be incubated 1.5 hours, reduce top heating unit, middle part heating unit and bottom heating unit temperature to 1100 ℃ with 2.5 hours again, be incubated 1.5 hours; Again by the temperature to 800 ℃ that reduces top heating unit, middle part heating unit and bottom heating unit in 2.5 hours, be incubated 0.5 hour afterwards.Finally close the power supply of heating unit, allow silicon ingot automatically lower the temperature.
(6) going out ingot finishes: when the temperature of the polycrystal silicon ingot formed when polysilicon is reduced to below 300 ℃, open bell 1, start rotatable lifting water cold platform mechanism 18, crucible 19 is risen to its bottom surface and exceed upper bell 1 oral thermometer face, take out polycrystalline silicon ingot casting, EO.
Through the experiment the data obtained, contrast as follows:
Embodiment 3:
A kind of process control method of polysilicon directional freezing, adopt device in embodiment 1, and preparation step is as follows:
(1) crucible of the quartzy material of Φ 900mm*600mm 19 is placed in body of heater, and is connected with rotatable lifting water cold platform mechanism 18, the 640kg silicon material of packing into.Crucible 19 is outer surrounds protection with the plumbago crucible backplate.
(2) rotatable lifting water cold platform mechanism 18 drives crucibles 19 and descends, and on closure, bell 1, starts to vacuumize.
(3) when the vacuum tightness of body of heater inside reaches 1Pa, beginning is to applying argon gas in body of heater, when the vacuum tightness of body of heater inside reaches 60000Pa, in startup, heating unit, middle heating unit and lower heating unit, start to heat silicon material 2, through 6 hours, silicon material 2 starts fusing, then continues heating after 4 hours, and the silicon material melts fully, now, be incubated 0.5 hour at the temperature of 1490 ℃.
According to following steps, proceed:
(4) the silicon body is long brilliant: the temperature that progressively reduces middle part heating unit and bottom heating unit, and improve the flow velocity of water in rotatable lifting water cold platform mechanism 18 simultaneously, crucible 19 bottom temps are reduced gradually, when crucible 19 bottom temps during lower than 1414 ℃, crucible 19 bottoms start crystallization and form polysilicon, when directional freeze to 45%, and then the temperature of reduction top heating unit, make polysilicon continue up growth.
The cooling of middle part heating unit and bottom heating unit is carried out according to following program: temperature is since 1500 ℃ of declines, and initial 3 hours with the per hour speed decline of 25 ℃, subsequently with the per hour speed decline of 15 ℃, until drop to 1000 ℃.
The cooling of top heating unit is carried out according to following program: since 1500 ℃ of declines, with the per hour speed decline of 5 ℃, finally be stabilized in 1370 ℃.
In rotatable lifting water cold platform mechanism 18, the flow velocity of water is 300L/min.
(5) anneal cooling: when polysilicon grows into fully, adjust top heating unit, middle part heating unit and bottom heating unit temperature, to the polycrystal silicon ingot rear insulation of being annealed, finally close the power supply of heating unit, allow silicon ingot automatically lower the temperature.
Wherein, step (5) is carried out in such a way: after polycrystal silicon ingot grows into fully, improve middle part heating unit and bottom heating unit to 1370 ℃, be incubated 2.5 hours, reduce top heating unit, middle part heating unit and bottom heating unit temperature to 1200 ℃ with 3.5 hours again, be incubated 2.5 hours; Again by the temperature to 950 ℃ that reduces top heating unit, middle part heating unit and bottom heating unit in 3.5 hours, be incubated 1.5 hours afterwards.Finally close the power supply of heating unit, allow silicon ingot automatically lower the temperature.
(6) going out ingot finishes: when the temperature of the polycrystal silicon ingot formed when polysilicon is reduced to below 300 ℃, open bell 1, start rotatable lifting water cold platform mechanism 18, crucible 19 is risen to its bottom surface and exceed upper bell 1 oral thermometer face, take out polycrystalline silicon ingot casting, EO.
Through the experiment the data obtained, contrast as follows:
Embodiment 4:
A kind of process control method of polysilicon directional freezing, adopt device in embodiment 1, and preparation step is as follows:
(1) crucible of the quartzy material of Φ 900mm*600mm 19 is placed in body of heater, and is connected with rotatable lifting water cold platform mechanism 18, the 650kg silicon material of packing into.Crucible 19 is outer surrounds protection with the plumbago crucible backplate.
(2) rotatable lifting water cold platform mechanism 18 drives crucibles 19 and descends, and on closure, bell 1, starts to vacuumize.
(3) when the vacuum tightness of body of heater inside reaches 1Pa, beginning is to applying argon gas in body of heater, when the vacuum tightness of body of heater inside reaches 60000Pa, in startup, heating unit, middle heating unit and lower heating unit, start to heat silicon material 2, through 6 hours, silicon material 2 starts fusing, then continues heating after 4 hours, and the silicon material melts fully, now, be incubated 0.5 hour at the temperature of 1490 ℃.
According to following steps, proceed:
(4) the silicon body is long brilliant: the temperature that progressively reduces middle part heating unit and bottom heating unit, and improve the flow velocity of water in rotatable lifting water cold platform mechanism 18 simultaneously, crucible 19 bottom temps are reduced gradually, when crucible 19 bottom temps during lower than 1414 ℃, crucible 19 bottoms start crystallization and form polysilicon, when directional freeze to 50%, and then the temperature of reduction top heating unit, make polysilicon continue up growth.
The cooling of middle part heating unit and bottom heating unit is carried out according to following program: temperature is since 1470 ℃ of declines, and initial 3 hours with the per hour speed decline of 20 ℃, subsequently with the per hour speed decline of 10 ℃, until drop to 980 ℃.
The cooling of top heating unit is carried out according to following program: since 1470 ℃ of declines, with the per hour speed decline of 3 ℃, finally be stabilized in 1360 ℃.
In rotatable lifting water cold platform mechanism 18, the flow velocity of water is 250L/min.
(5) anneal cooling: when polysilicon grows into fully, adjust top heating unit, middle part heating unit and bottom heating unit temperature, to the polycrystal silicon ingot rear insulation of being annealed, finally close the power supply of heating unit, allow silicon ingot automatically lower the temperature.
Wherein, step (5) is carried out in such a way: after polycrystal silicon ingot grows into fully, improve middle part heating unit and bottom heating unit to 1360 ℃, be incubated 2 hours, reduce top heating unit, middle part heating unit and bottom heating unit temperature to 1150 ℃ with 3 hours again, be incubated 2 hours; Again by the temperature to 870 ℃ that reduces top heating unit, middle part heating unit and bottom heating unit in 3 hours, be incubated 1 hour afterwards.Finally close the power supply of heating unit, allow silicon ingot automatically lower the temperature.
(6) going out ingot finishes: when the temperature of the polycrystal silicon ingot formed when polysilicon is reduced to below 300 ℃, open bell 1, start rotatable lifting water cold platform mechanism 18, crucible 19 is risen to its bottom surface and exceed upper bell 1 oral thermometer face, take out polycrystalline silicon ingot casting, EO.
Through the experiment the data obtained, contrast as follows:
Claims (5)
1. the process control method of a polysilicon directional freezing, first vacuumize, and then in body of heater, passes into argon gas, then, by silicon material heat fused, it is characterized in that proceeding according to following steps:
(1) the silicon body is long brilliant: the temperature that progressively reduces middle part heating unit and bottom heating unit, and improve the flow velocity of water in rotatable lifting water cold platform mechanism (18) simultaneously, crucible (19) bottom temp is reduced gradually, when crucible (19) bottom temp during lower than 1414 ℃, crucible (19) bottom starts crystallization and forms polysilicon, when directional freeze during to 45-55%, and then reduce the temperature of top heating unit, make polysilicon continue up growth;
(2) anneal cooling: when polysilicon grows into fully, adjust top heating unit, middle part heating unit and bottom heating unit temperature, to the polycrystal silicon ingot rear insulation of being annealed, finally close the power supply of heating unit, allow silicon ingot automatically lower the temperature;
(3) going out ingot finishes: when the temperature of the polycrystal silicon ingot formed when polysilicon is reduced to below 300 ℃, open bell (1), start rotatable lifting water cold platform mechanism (18), crucible is risen to its bottom surface and exceed body of heater upper flange surface, take out polycrystalline silicon ingot casting, EO.
2. the process control method of a kind of polysilicon directional freezing claimed in claim 1, it is characterized in that middle part heating unit in described step (1) and the cooling of bottom heating unit carry out according to following program: temperature is since 1450 ℃-1500 ℃ declines, initial 3 hours with the per hour speed decline of 15-25 ℃, subsequently with the per hour speed decline of 5-15 ℃, until drop to 950-1000 ℃.
3. the process control method of a kind of polysilicon directional freezing claimed in claim 1, the cooling that it is characterized in that the top heating unit in described step (1) is carried out according to following program: from 1460-1500 ℃, start to descend, with the per hour speed decline of 2-5 ℃, finally be stabilized in 1350-1370 ℃.
4. the process control method of a kind of polysilicon directional freezing claimed in claim 1, is characterized in that in described step (1), and in rotatable lifting water cold platform mechanism (18), the flow velocity of water is 200-300L/min.
5. the process control method of a kind of polysilicon directional freezing claimed in claim 1, it is characterized in that in described step (2) after polycrystal silicon ingot grows into fully, improve middle part heating unit and bottom heating unit to 1350-1370 ℃, insulation 1.5-2.5 hour, reduced top heating unit, middle part heating unit and bottom heating unit temperature to 1100-1200 ℃ with 2.5-3.5 hour again, insulation 1.5-2.5 hour; Use again afterwards the temperature that reduces top heating unit, middle part heating unit and bottom heating unit in 2.5-3.5 hour to 800-950 ℃, be incubated 0.5-1.5 hour, finally close the power supply of heating unit, allow silicon ingot automatically lower the temperature.
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Application publication date: 20131211 |