CN102330148B - Polysilicon ingot casting method with low defect and high output and thermal field structure thereof - Google Patents
Polysilicon ingot casting method with low defect and high output and thermal field structure thereof Download PDFInfo
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Abstract
The invention relates to a polysilicon ingot casting method with low defect and high output and a thermal field structure thereof. The thermal field structure comprises a thermal insulation cover system, a crucible system, split resistance heaters, a support part and a cooling device, wherein the three heaters are independently and separably controlled to lower energy consumption to the maximum degree and bring convenience for regulating a crystal growth interface, thereby obtaining an evener crystal growth interface, improving crystal quality and solving the later-stage cooling problem of the crystal growth because of the increase of the height of the ingot casting. A support block with the unique design and a cooling device are combined to realize the purpose of local cooling, so that the local position on the bottom of a crucible generates cold spots at the early stage of the crystal growth; nucleation is carried out firstly to reduce nucleation spots, and lateral temperature gradient is obtained to provide the necessary condition for the lateral growth of the crystal nucleus; crystalline grains are enlarged to reduce a crystal boundary to the large extent; and microdefects, such as dislocation and the like, are lowered.
Description
Technical field
The invention belongs to solar battery casting ingot technical field, relate to a kind of low defect high production polycrystalline silicon ingot casting method and thermal field structure thereof.
Background technology
In photovoltaic field, utilizing the method production polycrystal silicon ingot of directional freeze is the method generally adopting, and its ultimate principle is: polycrystalline silicon raw material is placed in quartz ceramic crucible, is placed in specific thermal field system, be heated to melt completely; Then from the bottom of crucible, begin to cool down, silicon solution starts crystallization in crucible bottom, gradually upwards growth (solidifying); Complete after process of growth, conventionally can thermal field is again closed, and begin to cool down after by one section of polycrystalline cast ingot insulation time, whole process energy consumption is in 3800 degree left and right.Energy consumption height is mainly that well heater is positioned at thermal field top and upper lateral part due to heater locations upper part at whole thermal field structure, and in order to maintain the thermograde of crystal growth, energy scatters and disappears more.In industry, generally adopt the 450kg polycrystalline cast ingot type of furnace at present, problem due to throughput or slicing machine load, actual charging capacity is generally at 390-420kg, development along with industry, compete more and more fierce, each manufacture of solar cells producer more and more focuses on the control to cost, in order to increase production capacity, reduce energy originally, various new equipment is constantly developed out, polycrystalline furnace has the larger type of furnace (800kg) to research and develop successfully, these large type of furnaces are all in past crosswise development, it is the original 450kg polycrystalline cast ingot type of furnace, can cut the fritter of 25 156mm * 156mm * 250mm, the 800kg type of furnace can cut out 36 such fritters, but the large-scale crucible production technique also prematurity supporting with it, and require larger excavation machine, original excavation machine is too narrow and can not continue to use, therefore its cost advantage is also not obvious.For improving output on original 450kg type of furnace basis, directly increase charge amount, along with the raising of charge amount, long brilliant later stage heat radiation difficulty, the long brilliant time significantly lengthens, and energy consumption increases.Simultaneously, polycrystalline silicon ingot casting is due to the problem of growth pattern, the bottom of quartz ceramic crucible first starts heat radiation, whole plane specific heat load is basically identical, crucible bottom produces many nucleation sites, and the crystal grain of generation is less, and crystal boundary and dislocation defect are higher, therefore compare with monocrystalline, institute's solar battery efficiency of doing can be low by 1%～2%.
Summary of the invention
The technical problem to be solved in the present invention is: propose a kind of low defect high production polycrystalline silicon ingot casting method and thermal field structure thereof, on current 450kg polycrystalline cast ingot type of furnace basis (still evolution 25 there emerged a the fritter of 156mm * 156mm), the charge amount Energy Intensity Reduction again that gets a promotion simultaneously, growth interface is controlled, and growing crystal, to grow into epipole less, and crystal grain is larger, the crystal ingot that crystal boundary and dislocation defect are little, section is for the production of solar cell, and battery efficiency can obtain obviously and promote.
The technical solution adopted in the present invention is: a kind of low defect high production polycrystalline silicon ingot casting method: the silicon material of 550-750kg is put into the crucible that 480-650mm is high, closed whole thermal field space, 3 resistance heaters of top and side heat simultaneously, wherein side heater is divided into upper and lower two parts, temperature is elevated to 1500 ℃ of left and right makes silicon material heat up and melt in more than ten hour, during material, keep pressure at 0.1-0.6atm, impurity in silicon material can be volatilized fully, pass into the inertia protective gas such as argon gas or helium simultaneously, impurity is easy to carry, after material finishes, promote the stay-warm case 0-60mm of sidewall, under side, heater heats power proportions is reduced to 0-50%, open the refrigerating unit under back-up block, with the back-up block of unique design and refrigerating unit, combine and realize Local cooling, make crucible bottom form local nucleation site at the long brilliant initial stage, in crucible bottom, form the thermograde of partial lateral, nucleus is toward transverse growth, form larger crystal grain, this period is controlled at 1-2h, complete the crystal grain expansion process at long brilliant initial stage.
Then close the refrigerating unit under back-up block, simultaneously again by the lifting of stay-warm case and the adjustment of 3 heater power ratios, strengthen bottom heat radiation, and silicon liquid needed hot environment in top is maintained by heater top and side upper heater, controlling long crystal boundary face moves on smooth, crystal is upwards growth gradually, so just form first horizontal after growth mechanism longitudinally.
In the long brilliant later stage, because solidifying, silico briquette there is thickness, and the thermal resistance effect meeting of silico briquette itself makes top silicon liquid heat radiation slack-off, long brilliant thermograde reduces, in order to shorten long brilliant saving of time energy consumption, can coordinate processing requirement again to open the refrigerating unit under back-up block, strengthen bottom heat radiation.The brilliant process of whole length completes in 20-35h.
After long crystalline substance finishes, close refrigerating unit, the while is closed whole stay-warm case again, under the high temperature of 1350 ℃, is incubated 1-6h, eliminates thermal stresses, and whole long crystalline substance and insulating process furnace pressure maintain 0.1-0.6atm.
After being incubated, open gradually again stay-warm case, make silicon ingot Slow cooling, now can increase gradually pressure to approaching 1atm, complete whole ingot casting process.
Meanwhile, the present invention also provides a kind of low defect high production polycrystalline silicon ingot casting thermal field structure of realizing the method, comprises stay-warm case system, crucible system, split type resistance well heater, support section, refrigerating unit.
Stay-warm case system comprises GRD geared stay-warm case sidewall and upper and lower warming plate, sidewall can move up and down, and upper and lower warming plate position is fixed, and stay-warm case is made by the lower insulation quilt of thermal conductivity, as graphite felt, suspension rod and support frame material are made by refractory metal.
Crucible system comprises quartz crucible, plumbago crucible, and plumbago crucible cover plate, cover plate is provided with shielding gas ingress pipe, and shielding gas is rare gas element.
Support section comprises graphite back-up block and 3 graphite support bars.The design of back-up block band hole or back-up block surface have the groove be arrangeding in parallel, as Local cooling point, use, and cooling point number can be 4-500.
Refrigerating unit is provided with cooling gas ingress pipe, combines and realizes Local cooling with back-up block.
Crucible system is placed on back-up block, crucible cover plate top has the heater top being connected on warming plate, crucible around has well heater under the side upper heater that is connected on warming plate and side, three well heaters can independently be controlled, heater top and help the distance between solidifying back-up block to reach 580-740mm, to load the silicon material of 550-750kg; Water cooler is arranged under back-up block; With upper-part, be all positioned at stay-warm case.
The invention has the beneficial effects as follows: realize larger charge amount 550-750kg silicon material, can improve the production capacity of ingot casting, the utilization ratio of crystal ingot, crystal ingot height can reach 340mm～465mm; Simultaneously because side heater is divided into two heating zone, can energy efficient, reduce whole ingot casting cost; The Local cooling effect of crucible bottom, make crucible bottom form less nucleation site at the long brilliant initial stage, in crucible bottom, form the thermograde of partial lateral, nucleus is toward transverse growth, form larger crystal grain, and then by the lifting of heat-insulation cage and the adjustment of side two well heaters, bottom heat radiation strengthens, control long crystal boundary face and move on smooth, crystal is upwards growth gradually.Growth mechanism longitudinally after so forming first laterally, thus crystal boundary and dislocation significantly reduce, and crystal mass increases substantially.Adopt the present invention, unit time output can improve 15%～40%, unit output Energy Intensity Reduction 10%～40%, and the defective proportion such as grain boundary dislocation reduce more than 50%.
Compare with current existing technology, side heater is divided into two heating zone, adds the well heater of upper top, 3 well heaters can separate independent control, can reduce to the full extent energy consumption, and are beneficial to the long crystal boundary face of adjusting, obtain more smooth long crystal boundary face, improve crystal mass; With the back-up block of unique design and refrigerating unit, combine and realize Local cooling, make to produce cold spot at long brilliant initial stage crucible bottom local location, first start forming core, reduced nucleation site, and obtained horizontal thermograde, for nucleus, laterally grown up essential condition is provided.The present invention has significantly lifting on stocking space, the height of ingot casting reaches 340mm～465mm (the general ingot height of existing ingot furnace 250mm), due to the thermal resistance problem of the silico briquette growing own, make long brilliant later stage heat radiation difficulty, and the refrigerating unit of back-up block of the present invention bottom also can be adjusted the heat radiation in long brilliant later stage, heat is distributed sooner, maintain the needed thermograde of long brilliant interface displacement, solved the heat dissipation problem bringing due to the increase of ingot height.
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the present invention is further described.
Fig. 1 is the schematic diagram of thermal field structure of the present invention;
Fig. 2 is a kind of schematic diagram of the hole design of graphite back-up block of the present invention;
Fig. 3 is the another kind of structural representation of the hole design of graphite back-up block of the present invention;
In figure: 1, upper warming plate; 2, heater top; 3, side upper heater; 4, well heater under side; 5, stay-warm case sidewall; 6, plumbago crucible; 7, back-up block; 8, refrigerating unit; 9, upper warming plate; 10 support bars; 11, cooling gas ingress pipe; 12, quartz crucible; 13, crucible cover plate; 14, shielding gas ingress pipe.
Embodiment
The present invention is further detailed explanation with preferred embodiment by reference to the accompanying drawings now.These accompanying drawings are the schematic diagram of simplification, basic structure of the present invention is only described in a schematic way, so it only show the formation relevant with the present invention.
A kind of low defect high production polycrystalline silicon ingot casting thermal field structure as shown in Figure 1, comprise GRD geared stay-warm case sidewall 5 and upper warming plate 1, lower warming plate 9 and graphite back-up block 7 with graphite support bar 10, quartz crucible 12 on back-up block 7 in placing graphite crucible 6 and plumbago crucible, on crucible, be provided with cover plate 13, cover plate is provided with inert protective gas ingress pipe 14, crucible cover plate top also has the heater top 2 being connected on warming plate 1, crucible around has well heater 4 under the side upper heater 3 that is connected on warming plate 1 and side, 3 side well heaters can independently be controlled, heater top and help the distance between solidifying back-up block to reach 580-740mm, to load the silicon material of 550-750kg, water cooler arranges 8 back-up block 7 times, back-up block 7 band hole designs: as Fig. 2,3, use as Local cooling point, cooling point number can be 4-500, and figure only, for signal, is not limited to above-mentioned hole proterties.Water cooler is provided with cooling gas ingress pipe 11, combines and realizes Local cooling with back-up block.
Embodiment 1
Quartz crucible 12 is filled after 650kg silicon material, outsourcing plumbago crucible 6, be positioned on back-up block 7, stay-warm case sidewall 5 and lower warming plate 9 closures, distance between heater top 2 and back-up block 7 reaches 650mm, body of heater is vacuumized, reach after processing requirement vacuum tightness, heater top 2, under side upper heater 3 and side, well heater 4 is started working, after preliminary preheating, by shielding gas ingress pipe 14, pass into gradually inert protective gas argon gas, maintain furnace pressure 0.5atm, insulation effect due to stay-warm case, temperature in stay-warm case can be elevated to the high temperature of 1500 ℃ of left and right, make silicon material heat up and melt in more than ten hour.The impurity that the argon gas portability material circulating during material evaporates, material finishes rear stable 1h, promote the stay-warm case 30mm of sidewall, under side, heater heats power proportions is reduced to 50%, open the refrigerating unit 8 under back-up block, by cooling gas ingress pipe 11, import cooling gas, back-up block 7 is with 25 cooling points, as Fig. 2, back-up block 7 and refrigerating unit 8 are combined and are realized Local cooling, make quartz crucible 12 bottoms form local nucleation site at the long brilliant initial stage, in crucible bottom, form the thermograde of partial lateral, nucleus is toward transverse growth, form larger crystal grain, this period is controlled at 1-2h, complete the crystal grain expansion process at long brilliant initial stage.Then close the refrigerating unit 8 under back-up block, cooling gas ingress pipe 11 stops importing cooling gas, again by the lifting of stay-warm case and the adjustment of 3 heater power ratios, strengthen bottom heat radiation, and silicon liquid needed hot environment in top is maintained by heater top 2 and side upper heater 3, make the crystalizing interface of silicon form a vertical temperature gradient field, control long crystal boundary face and move on smooth, crystal is upwards growth gradually, so just form first horizontal after growth mechanism longitudinally.It is given that the data that thermodynamical model gathers according to automatic control system are carried out the set(ting)value of temperature distribution, and the set(ting)value that automatic control system distributes according to given temperature space is controlled well heater.
In the long brilliant later stage, because solidifying, silico briquette there is thickness, and the thermal resistance effect meeting of silico briquette itself makes top silicon liquid heat radiation slack-off, long brilliant thermograde reduces, in order to shorten long brilliant saving of time energy consumption, can coordinate processing requirement again to open the refrigerating unit 8 under back-up block 7, strengthen bottom heat radiation.The brilliant process of whole length completes in 28h.
After long crystalline substance finishes, close refrigerating unit 8, the while is closed whole stay-warm case again, under the high temperature of 1350 ℃, is incubated 3h, eliminates thermal stresses, and whole process furnace pressure maintains 0.5atm.
After being incubated, open gradually again stay-warm case, make silicon ingot Slow cooling in 12h, now can increase gradually the nearly 1atm of pressure reverse graft, complete whole ingot casting process.Institute goes out the high 406mm of ingot, and output increases by 60%, unit output Energy Intensity Reduction 30%, and silicon ingot grain size increases to 3-10cm by original 1-3cm, grain boundary dislocation etc., and microdefect reduces more than 50%.
Embodiment 2
Quartz crucible 12 is filled after 750kg silicon material, outsourcing plumbago crucible 6, be positioned on back-up block 7, stay-warm case sidewall 5 and lower warming plate 9 closures, distance between heater top 2 and back-up block 7 reaches 700mm, body of heater is vacuumized, reach after processing requirement vacuum tightness, heater top 2, under side upper heater 3 and side, well heater 4 is started working, after preliminary preheating, by shielding gas ingress pipe 14, pass into gradually inert protective gas argon gas, maintain furnace pressure 0.6atm, insulation effect due to stay-warm case, temperature in stay-warm case can be elevated to the high temperature of 1500 ℃ of left and right, make silicon material heat up and melt in more than ten hour.The impurity that the argon gas portability material circulating during material evaporates, material finishes rear stable 1h, under side, heater heats power proportions is reduced to 30%, open the refrigerating unit 8 under back-up block, by cooling gas ingress pipe 11, import cooling gas, back-up block 7 is with 4 strip cooling points, as Fig. 3, back-up block 7 and refrigerating unit 8 are combined and are realized Local cooling, make quartz crucible 12 bottoms form local nucleation site at the long brilliant initial stage, in crucible bottom, form the thermograde of partial lateral, nucleus is toward transverse growth, form larger crystal grain, this period is controlled at 1-2h, complete the crystal grain expansion process at long brilliant initial stage.Then close the refrigerating unit 8 under back-up block, cooling gas ingress pipe 11 stops importing cooling gas, again by the lifting of stay-warm case and the adjustment of 3 heater power ratios, strengthen bottom heat radiation, and silicon liquid needed hot environment in top is maintained by heater top 2 and side upper heater 3, make the crystalizing interface of silicon form a vertical temperature gradient field, control long crystal boundary face and move on smooth, crystal is upwards growth gradually, so just form first horizontal after growth mechanism longitudinally.It is given that the data that thermodynamical model gathers according to automatic control system are carried out the set(ting)value of temperature distribution, and the set(ting)value that automatic control system distributes according to given temperature space is controlled well heater.
In the long brilliant later stage, because solidifying, silico briquette there is thickness, and the thermal resistance effect meeting of silico briquette itself makes top silicon liquid heat radiation slack-off, long brilliant thermograde reduces, in order to shorten long brilliant saving of time energy consumption, can coordinate processing requirement again to open the refrigerating unit 8 under back-up block 7, strengthen bottom heat radiation.The brilliant process of whole length completes in 30h.
After long crystalline substance finishes, close refrigerating unit 8, the while is closed whole stay-warm case again, under the high temperature of 1375 ℃, is incubated 4h, eliminates thermal stresses, and whole process furnace pressure maintains 0.6atm.
After being incubated, open gradually again stay-warm case, make silicon ingot Slow cooling in 12h, now can increase gradually the nearly 1atm of pressure reverse graft, complete whole ingot casting process.Institute goes out the high 465mm of ingot, and output increases by 80%, unit output Energy Intensity Reduction 35%, and silicon ingot grain size increases to 3-10cm by original 1-3cm, grain boundary dislocation etc., and microdefect reduces more than 50%.
In the long brilliant later stage, because solidifying, silico briquette there is thickness, and the thermal resistance effect meeting of silico briquette itself makes top silicon liquid heat radiation slack-off, long brilliant thermograde reduces, in order to shorten long brilliant saving of time energy consumption, can coordinate processing requirement again to open the refrigerating unit 8 under back-up block 7, strengthen bottom heat radiation.The brilliant process of whole length completes in 28h.
After long crystalline substance finishes, close refrigerating unit 8, the while is closed whole stay-warm case again, under the high temperature of 1375 ℃, is incubated 4h, eliminates thermal stresses, and whole process furnace pressure maintains 0.4atm.
After being incubated, open gradually again stay-warm case, make silicon ingot Slow cooling in 12h, now can increase gradually the nearly 1atm of pressure reverse graft, complete whole ingot casting process.Institute goes out the high 406mm of ingot, and output increases by 60%, unit output Energy Intensity Reduction 30%, and silicon ingot, by the more polycrystalline of the mixed and disorderly crystal grain of original direction, becomes and possesses unified crystal orientation, grain boundary dislocation etc., and microdefect reduces more than 60%.
Just the specific embodiment of the present invention of describing in above specification sheets, various not illustrating is construed as limiting flesh and blood of the present invention, person of an ordinary skill in the technical field read after specification sheets can to before described embodiment make an amendment or be out of shape, and do not deviate from essence of an invention and scope.
Claims (6)
1. a low defect high production polycrystalline silicon ingot casting method, is characterized in that comprising the following steps:
1) the silicon material of 550-750kg is put into the crucible that 480-650mm is high, closed whole thermal field space, 3 resistance heaters of top and side heat simultaneously, and wherein side heater is divided into upper and lower two parts; Temperature is elevated to 1500 ℃, makes silicon material heat up and melt in more than ten hour, keeps pressure at 0.1-0.6atm during material, passes into inertia protective gas simultaneously; After material finishes, promote the stay-warm case 0-60mm of sidewall, under side, heater heats power proportions is reduced to 0-50%, opens the refrigerating unit under back-up block, utilizes back-up block and refrigerating unit to combine and realizes Local cooling, make crucible bottom form local nucleation site at the long brilliant initial stage, in crucible bottom, form the thermograde of partial lateral, nucleus, toward transverse growth, forms larger crystal grain, this period is controlled at 1-2h, completes the crystal grain expansion process at long brilliant initial stage;
2) close the refrigerating unit under back-up block, simultaneously again by the lifting of stay-warm case and the adjustment of 3 heater power ratios, strengthen bottom heat radiation, and silicon liquid needed hot environment in top is maintained by heater top and side upper heater, controlling long crystal boundary face moves on smooth, crystal is upwards growth gradually, form first laterally after growth mechanism longitudinally;
3) in the long brilliant later stage, coordinate processing requirement again to open the refrigerating unit under back-up block, strengthen bottom heat radiation, the brilliant process of whole length completes in 20-35h;
4) long crystalline substance is closed refrigerating unit after finishing, and the while is closed whole stay-warm case again, under the high temperature of 1350 ℃, is incubated 1-6h, eliminates thermal stresses, and whole long crystalline substance and insulating process furnace pressure maintain 0.1-0.6atm; After being incubated, open gradually again stay-warm case, make silicon ingot Slow cooling, increase gradually pressure to approaching 1atm, complete whole ingot casting process.
2. a low defect high production polycrystalline silicon ingot casting thermal field structure, is characterized in that: comprise GRD geared stay-warm case sidewall (5) and upper warming plate (1), lower warming plate (9) and the graphite back-up block (7) of band graphite support bar (10); Quartz crucible (12) in the upper placing graphite crucible (6) of described back-up block (7) and plumbago crucible, on plumbago crucible, be provided with cover plate (13), cover plate is provided with inert protective gas ingress pipe (14), crucible cover plate top also has the heater top (2) being connected on warming plate (1), described crucible around has well heater (4) under the side upper heater (3) that is connected on warming plate (1) and side, 3 well heaters are independently controlled, and the distance between heater top and back-up block is 580-740mm; Refrigerating unit (8) is arranged under back-up block (7); The hole design of back-up block (7) band or back-up block (7) surface have the groove be arrangeding in parallel; Refrigerating unit (8) is provided with cooling gas ingress pipe (11), combines and realizes Local cooling with back-up block (7).
3. low defect high production polycrystalline silicon ingot casting thermal field structure as claimed in claim 2, is characterized in that: the hole of described back-up block (7) is designed to the hole that described back-up block surface has a plurality of one-tenth arranged.
4. low defect high production polycrystalline silicon ingot casting thermal field structure as claimed in claim 2, is characterized in that: described refrigerating unit (8) is block or is arranged and formed by pipeline.
5. low defect high production polycrystalline silicon ingot casting thermal field structure as claimed in claim 3, is characterized in that: the number of the hole on described back-up block (7) is 4-500.
6. low defect high production polycrystalline silicon ingot casting thermal field structure as claimed in claim 2, is characterized in that: in corresponding Local cooling position, place seed crystal and realize monocrystalline induced growth effect.
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