CN104120492A - Manufacturing process of efficient semi-molten polycrystalline ingot casting - Google Patents
Manufacturing process of efficient semi-molten polycrystalline ingot casting Download PDFInfo
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- CN104120492A CN104120492A CN201410400824.8A CN201410400824A CN104120492A CN 104120492 A CN104120492 A CN 104120492A CN 201410400824 A CN201410400824 A CN 201410400824A CN 104120492 A CN104120492 A CN 104120492A
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Abstract
The invention relates to a manufacturing process of an efficient semi-molten polycrystalline ingot casting. The manufacturing process is characterized by comprising the following steps: (1) adopting the following raw materials in percentage by weight: 60-70% of primary polysilicon and 30-40% of polycrystalline auxiliary material; (2) putting the raw materials into a crucible, conveying the crucible into an ingot furnace, and putting the crucible on a DS block; positioning the crucible on the DS block, and covering a heater on the crucible, wherein the upper part of the heater is an upper heat insulation cage, and the lower part of the DS block is a lower heat preservation layer; (3) performing a five-step heating process; (4) performing a thirteen-step melting process; (5) performing a nine-step crystal growth process; (6) after annealing and cooling, when the temperature of an ingot furnace cavity is less than 400 DEG C, introducing argon into the furnace, and opening the ingot furnace when reaching 980mbar to obtain the polycrystalline ingot casting. The manufacturing process disclosed by the invention can be used for improving the whole ingot conversion efficiency, and is low in cost.
Description
Technical field
The present invention relates to a kind of manufacture craft of efficient fritting polycrystalline cast ingot, belong to photovoltaic technology field.
Background technology
Along with the development of world economy, energy problem and environmental problem seem more and more important, are directly connected to socioeconomic Sustainable development.The starting material such as life-time service coal and oil can bring serious pollution to environment as the energy.Therefore developing renewable and clean energy resource just becomes a kind of very important approach.Sun power is most important clean renewable energy source, and for the exploitation of sun power, World Developed Countries gives the attention of height.Within 2014, world environment day China slogan is " to polluting challenge ", and its object is exactly for low-carbon green environmental protection, makes sky more blue, and water is more clear, and everybody lives among a harmonious atmosphere of not polluting.
The photoelectric transformation efficiency of solar battery sheet is just to weigh quality product quality sole criterion, and current domestic P type single-chip efficiency of conversion is generally more than 18%, and N-type efficiency of conversion can reach more than 20%.But single crystal battery sheet manufacturing cost is high, reason is high to starting material requirement, and equipment manufacturing cost is high, complicated operation, and qualification rate is low, has caused like this single crystal battery sheet cost expensive more a lot of than polycrystalline.And polycrystalline has certain tolerance to starting material, and along with the increasing of charging capacity, produce a stove polycrystalline ingot and can go out a lot of cell pieces, production efficiency significantly improves like this, cost a lot.From current present situation, casting polycrystalline silicon material has been substituted pulling of crystals silicon materials becomes topmost solar cell material, but the competition in market impels the production technique of casting polycrystalline silicon material constantly to reform, low-cost and high-level efficiency is two basic conditions that photovoltaic worker is able to long-time Sustainable development.Be engaged in the recent period sun power research staff research focus is focused in polycrystalline cell piece efficiency of conversion, can catch up with or approach single crystal battery sheet efficiency of conversion becomes the large problem of researcher one.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of manufacture craft of efficient fritting polycrystalline cast ingot is provided, improve whole ingot efficiency of conversion, and cost is low.
According to technical scheme provided by the invention, the manufacture craft of described efficient fritting polycrystalline cast ingot, feature is to comprise the following steps:
(1) raw material: primary polysilicon 60～70%, polycrystalline auxiliary material 30～40%;
(2) raw material is encased in crucible, crucible is sent in ingot furnace, be positioned on DS piece; Crucible is positioned on DS piece, and crucible upper cover is established well heater, and well heater outside is upper heat-insulation cage, and DS piece bottom is lower thermal insulation layer;
(3) heat-processed comprises following 5 steps:
The 1st step: be 10～15min heat-up time, Heating temperature is 150～200 ℃, vacuum tightness is 0.02～0.006mbar;
The 2nd step: be 30～40min heat-up time, Heating temperature is 400～450 ℃, vacuum tightness is 0.02～0.006mbar;
The 3rd step: be 90～100min heat-up time, Heating temperature is 700～800 ℃, vacuum tightness is 0.02～0.006mbar;
The 4th step: be 120～130min heat-up time, Heating temperature is 1100～1175 ℃, vacuum tightness is 0.02～0.006mbar;
The 5th step: be 150～155min heat-up time, Heating temperature is 1170～1175 ℃, vacuum tightness is 0.02～0.006mbar;
(4) melting process comprises following 13 steps:
The 1st step: be 30～35min heat-up time, Heating temperature is 1175～1180 ℃, ingot furnace cavity pressure set(ting)value is 0.02～0.006 mbar;
The 2nd step: be 12～15min heat-up time, Heating temperature is 1193～1195 ℃, logical argon gas, ingot furnace cavity pressure is 190～195 mbar;
The 3rd step: be 12～15min heat-up time, Heating temperature is 1210～1215 ℃, logical argon gas, ingot furnace cavity pressure 350～355mbar;
The 4th step: be 180～185min heat-up time, Heating temperature is 1455～1460 ℃, logical argon gas, ingot furnace cavity pressure is 500～505 mbar;
The 5th step: be 90～95min heat-up time, Heating temperature is 1500～1505 ℃, logical argon gas, ingot furnace cavity pressure is 550～555 mbar;
The 6th step: be 240～245min heat-up time, Heating temperature is 1540～1545 ℃, logical argon gas, ingot furnace cavity pressure is 550～555mbar;
The 7th step: be 720～725min heat-up time, Heating temperature is 1538～1540 ℃, logical argon gas, ingot furnace cavity pressure is 550～555 mbar, upper is 0.6～0.8cm every cage valve lift;
The 8th step: be 30～35min heat-up time, Heating temperature is 1532～1535 ℃, logical argon gas, ingot furnace cavity pressure is 550～555 mbar, upper every cage valve lift maintenance 0.6～0.8cm; ;
The 9th step: be 30～35min heat-up time, Heating temperature is 1480～1485 ℃, logical argon gas, ingot furnace cavity pressure is 550～555 mbar, upper every cage valve lift maintenance 0.6～0.8cm;
The 10th step: be 90～95min heat-up time, Heating temperature is 1445～1448 ℃, logical argon gas, ingot furnace cavity pressure is 550～555 mbar, upper every cage valve lift maintenance 0.6～0.8cm;
The 11st step: be 15～18min heat-up time, Heating temperature is 1445～1448 ℃, logical argon gas, ingot furnace cavity pressure is 550～555 mbar, upper is 6～8cm every cage valve lift;
(5) grow brilliant process and comprise following 9 steps:
The 1st step: be 180～185min heat-up time, Heating temperature is 1445～1448 ℃, logical argon gas, ingot furnace cavity pressure is 550～555mbar;
The 2nd step: be 180～182min heat-up time, Heating temperature is 1443～1444 ℃, logical argon gas, ingot furnace cavity pressure is 550～555 mbar;
The 3rd step: be 60～65min heat-up time, Heating temperature is 1442～1443 ℃, logical argon gas, ingot furnace cavity pressure is 550～555mbar;
The 4th step: be 300～305min heat-up time, Heating temperature is 1435～1438 ℃, logical argon gas, ingot furnace cavity pressure is 550～555 mbar;
The 5th step: be 480～485min heat-up time, Heating temperature is 1424～1425 ℃, logical argon gas, ingot furnace cavity pressure is 550～555 mbar;
The 6th step: be 240～245min heat-up time, Heating temperature is 1421～1423 ℃, logical argon gas, ingot furnace cavity pressure is 550～555mbar;
The 7th step: heat-up time 480～485min, Heating temperature is 1419～1421 ℃, logical argon gas, ingot furnace cavity pressure is 550～555mbar;
The 8th step: be 210～215min heat-up time, Heating temperature is 1418～1420 ℃, logical argon gas, ingot furnace cavity pressure is 550～555 mbar;
(6) annealing process: be 225～230min heat-up time, Heating temperature is 1370 ℃, logical argon gas, ingot furnace cavity pressure is 600～605 mbar;
(7) coolingly comprise following 5 steps:
The 1st step: be 180～185min cooling time, temperature is 1100～1370 ℃, logical argon gas, ingot furnace cavity pressure is 600～610mbar;
The 2nd step: be 180～185min cooling time, temperature is 800～1100 ℃, logical argon gas, ingot furnace cavity pressure is 600～610mbar;
The 3rd step: be 90～95min cooling time, temperature is 600～800 ℃, logical argon gas, ingot furnace cavity pressure is 700～710mbar;
The 4th step: be 360～365min cooling time, temperature is 410～600 ℃, logical argon gas, ingot furnace cavity pressure is 700～710 mbar;
The 5th step: be 20～25min cooling time, temperature is 390～410 ℃, logical argon gas, ingot furnace cavity pressure is 850～860mbar;
After upper cooling completing, ingot furnace cavity temperature is during lower than 400 ℃, when applying argon gas in stove reaches 980mbar, can open ingot furnace, obtains polycrystalline cast ingot.
Described polycrystalline auxiliary material is one or more in broken polycrystalline, polycrystalline flaw-piece, polycrystal tail, monocrystalline tailing, polycrystalline head material.
Described DS piece is all around around 4.5cm thickness insulation quilt.
The polycrystalline cast ingot efficiency of conversion that the manufacture craft of efficient fritting polycrystalline cast ingot of the present invention obtains reaches 17.6%; Bottom polycrystalline crystalline substance is spent evenly, and dislocation is few, and lattice defect is few.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention.
Embodiment
Below in conjunction with concrete accompanying drawing, the invention will be further described.
As shown in Figure 1: crucible 1 is positioned on DS piece 2, crucible 1 upper cover is established well heater 3, and well heater 3 outsides are upper heat-insulation cage 4, and DS piece 2 bottoms are lower thermal insulation layer 5; Principle of heating of the present invention is: top and the surrounding of 3 pairs of crucibles 1 of well heater heat, and the fusing order of the silicon material in crucible 1, is controlled bottom seed crystal and not exclusively melted to center for from top to bottom, by corner; In the fusion stage, temperature arrives 1400 ℃ when above, and upper heat-insulation cage 4 slowly opens to 6～8cm step by step, and by DS piece 2 all around around 4.5cm thickness insulation quilt to control bottom DS piece 2 temperature; This kind of method do not melt by control center region, make bottom silicon liquid form fast nucleus crossing when cold, guarantee corner and central zone temperature decline consistence (melted silicon panel region temperature is not between 1420 ℃ of left and right), thereby guarantee that bottom polycrystalline crystalline substance spends evenly, dislocation is few, and lattice defect is few.
Embodiment mono-: a kind of manufacture craft of efficient fritting polycrystalline cast ingot, comprises the following steps:
(1) raw material: primary polysilicon 60%, polycrystalline auxiliary material 40%; Polycrystalline auxiliary material is one or more in broken polycrystalline, polycrystalline flaw-piece, polycrystal tail, monocrystalline tailing, polycrystalline head material;
(2) raw material is encased in crucible, crucible is sent in ingot furnace, be positioned on DS piece (heat exchange mass);
(3) heat-processed comprises following 5 steps:
The 1st step: be 10min heat-up time, Heating temperature is 200 ℃, vacuum tightness is 0.02mbar;
The 2nd step: be 30min heat-up time, Heating temperature is 450 ℃, vacuum tightness is 0.02mbar;
The 3rd step: be 90min heat-up time, Heating temperature is 800 ℃, vacuum tightness is 0.02mbar;
The 4th step: be 120min heat-up time, Heating temperature is 1175 ℃, vacuum tightness is 0.02mbar;
The 5th step: be 150min heat-up time, Heating temperature is 1175 ℃, vacuum tightness is 0.02mbar;
(4) melting process comprises following 13 steps:
The 1st step: be 30min heat-up time, Heating temperature is 1180 ℃, ingot furnace cavity pressure set(ting)value is 0.02mbar;
The 2nd step: be 12min heat-up time, Heating temperature is 1195 ℃, logical argon gas, ingot furnace cavity pressure is 190mbar;
The 3rd step: be 12min heat-up time, Heating temperature is 1215 ℃, logical argon gas, ingot furnace cavity pressure 350mbar;
The 4th step: be 180min heat-up time, Heating temperature is 1460 ℃, logical argon gas, ingot furnace cavity pressure is 500mbar;
The 5th step: be 90min heat-up time, Heating temperature is 1505 ℃, logical argon gas, ingot furnace cavity pressure is 550mbar;
The 6th step: be 240min heat-up time, Heating temperature is 1545 ℃, logical argon gas, ingot furnace cavity pressure is 550 mbar;
The 7th step: be 720min heat-up time, Heating temperature is 1540 ℃, logical argon gas, ingot furnace cavity pressure is 550 mbar, upper is 0.6cm every cage valve lift;
The 8th step: be 30min heat-up time, Heating temperature is 1535 ℃, logical argon gas, ingot furnace cavity pressure is 550 mbar, upper every cage valve lift maintenance 0.6cm; ;
The 9th step: be 30min heat-up time, Heating temperature is 1485 ℃, logical argon gas, ingot furnace cavity pressure is 550mbar, upper every cage valve lift maintenance 0.6cm;
The 10th step: be 90min heat-up time, Heating temperature is 1448 ℃, logical argon gas, ingot furnace cavity pressure is 550mbar, upper every cage valve lift maintenance 0.6cm;
The 11st step: be 15min heat-up time, Heating temperature is 1448 ℃, logical argon gas, ingot furnace cavity pressure is 550mbar, upper is 6cm every cage valve lift;
(5) grow brilliant process and comprise following 9 steps:
The 1st step: be 180min heat-up time, Heating temperature is 1448 ℃, logical argon gas, ingot furnace cavity pressure is 550mbar;
The 2nd step: be 180min heat-up time, Heating temperature is 1444 ℃, logical argon gas, ingot furnace cavity pressure is 550mbar;
The 3rd step: be 60min heat-up time, Heating temperature is 1443 ℃, logical argon gas, ingot furnace cavity pressure is 550mbar;
The 4th step: be 300min heat-up time, Heating temperature is 1438 ℃, logical argon gas, ingot furnace cavity pressure is 550 mbar;
The 5th step: be 480min heat-up time, Heating temperature is 1425 ℃, logical argon gas, ingot furnace cavity pressure is 550mbar;
The 6th step: be 240min heat-up time, Heating temperature is 1423 ℃, logical argon gas, ingot furnace cavity pressure is 550mbar;
The 7th step: heat-up time 480min, Heating temperature is 1421 ℃, logical argon gas, ingot furnace cavity pressure is 550mbar;
The 8th step: be 210min heat-up time, Heating temperature is 1420 ℃, logical argon gas, ingot furnace cavity pressure is 550mbar;
(6) annealing process: be 225min heat-up time, Heating temperature is 1370 ℃, logical argon gas, ingot furnace cavity pressure is 600mbar;
(7) coolingly comprise following 5 steps:
The 1st step: be 180min cooling time, temperature is 1370 ℃, logical argon gas, ingot furnace cavity pressure is 600mbar;
The 2nd step: be 180min cooling time, temperature is 100 ℃, logical argon gas, ingot furnace cavity pressure is 600mbar;
The 3rd step: be 90min cooling time, temperature is 800 ℃, logical argon gas, ingot furnace cavity pressure is 700mbar;
The 4th step: be 360min cooling time, temperature is 600 ℃, logical argon gas, ingot furnace cavity pressure is 700mbar;
The 5th step: be 20min cooling time, temperature is 410 ℃, logical argon gas, ingot furnace cavity pressure is 850mbar;
After cooling the completing of above-mentioned 5 steps, ingot furnace cavity temperature is during lower than 400 ℃, when applying argon gas in stove reaches 980mbar, can open ingot furnace; With dummy car, inserting with the crucible of ingot casting, out deliver to indoor regulation place and naturally cool to room temp, the square ingot of pulling down after crucible 1 meter of square height and be 325 centimetres has been made into, and carries out evolution, flour milling, section and finally makes cell piece.
Embodiment bis-: a kind of manufacture craft of efficient fritting polycrystalline cast ingot, comprises the following steps:
(1) raw material: primary polysilicon 70%, polycrystalline auxiliary material 30%; Polycrystalline auxiliary material is one or more in broken polycrystalline, polycrystalline flaw-piece, polycrystal tail, monocrystalline tailing, polycrystalline head material;
(2) raw material is encased in crucible, crucible is sent in ingot furnace, be positioned on DS piece (heat exchange mass);
(3) heat-processed comprises following 5 steps:
The 1st step: be 15min heat-up time, Heating temperature is 150 ℃, vacuum tightness is 0.006mbar;
The 2nd step: be 40min heat-up time, Heating temperature is 400 ℃, vacuum tightness is 0.006mbar;
The 3rd step: be 100min heat-up time, Heating temperature is 700 ℃, vacuum tightness is 0.006mbar;
The 4th step: be 130min heat-up time, Heating temperature is 1100 ℃, vacuum tightness is 0.006mbar;
The 5th step: be 155min heat-up time, Heating temperature is 1170 ℃, vacuum tightness is 0.006mbar;
(4) melting process comprises following 13 steps:
The 1st step: be 35min heat-up time, Heating temperature is 1175 ℃, ingot furnace cavity pressure set(ting)value is 0.006 mbar;
The 2nd step: be 15min heat-up time, Heating temperature is 1193 ℃, logical argon gas, ingot furnace cavity pressure is 195 mbar;
The 3rd step: be 15min heat-up time, Heating temperature is 1210 ℃, logical argon gas, ingot furnace cavity pressure 355mbar;
The 4th step: be 185min heat-up time, Heating temperature is 1455 ℃, logical argon gas, ingot furnace cavity pressure is 505 mbar;
The 5th step: be 95min heat-up time, Heating temperature is 1500 ℃, logical argon gas, ingot furnace cavity pressure is 555 mbar;
The 6th step: be 245min heat-up time, Heating temperature is 1540 ℃, logical argon gas, ingot furnace cavity pressure is 555mbar;
The 7th step: be 725min heat-up time, Heating temperature is 1538 ℃, logical argon gas, ingot furnace cavity pressure is 555 mbar, upper is 0.8cm every cage valve lift;
The 8th step: be 35min heat-up time, Heating temperature is 1532 ℃, logical argon gas, ingot furnace cavity pressure is 555 mbar, upper every cage valve lift maintenance 0.8cm; ;
The 9th step: be 35min heat-up time, Heating temperature is 1480 ℃, logical argon gas, ingot furnace cavity pressure is 550mbar, upper every cage valve lift maintenance 0.8cm;
The 10th step: be 95min heat-up time, Heating temperature is 1445 ℃, logical argon gas, ingot furnace cavity pressure is 555 mbar, upper every cage valve lift maintenance 0.8cm;
The 11st step: be 18min heat-up time, Heating temperature is 1445 ℃, logical argon gas, ingot furnace cavity pressure is 555 mbar, upper is 8cm every cage valve lift;
(5) grow brilliant process and comprise following 9 steps:
The 1st step: be 1185min heat-up time, Heating temperature is 1445 ℃, logical argon gas, ingot furnace cavity pressure is 555mbar;
The 2nd step: be 182min heat-up time, Heating temperature is 1443 ℃, logical argon gas, ingot furnace cavity pressure is 555 mbar;
The 3rd step: be 65min heat-up time, Heating temperature is 1442 ℃, logical argon gas, ingot furnace cavity pressure is 555mbar;
The 4th step: be 305min heat-up time, Heating temperature is 1435 ℃, logical argon gas, ingot furnace cavity pressure is 555 mbar;
The 5th step: be 485min heat-up time, Heating temperature is 1424 ℃, logical argon gas, ingot furnace cavity pressure is 555 mbar;
The 6th step: be 245min heat-up time, Heating temperature is 1421 ℃, logical argon gas, ingot furnace cavity pressure is 555mbar;
The 7th step: heat-up time 485min, Heating temperature is 1419 ℃, logical argon gas, ingot furnace cavity pressure is 555mbar;
The 8th step: be 215min heat-up time, Heating temperature is 1418 ℃, logical argon gas, ingot furnace cavity pressure is 555 mbar;
(6) annealing process: be 230min heat-up time, Heating temperature is 1370 ℃, logical argon gas, ingot furnace cavity pressure is 605 mbar;
(7) coolingly comprise following 5 steps:
The 1st step: be 185min cooling time, temperature is 1100 ℃, logical argon gas, ingot furnace cavity pressure is 610mbar;
The 2nd step: be 185min cooling time, temperature is 800 ℃, logical argon gas, ingot furnace cavity pressure is 610mbar;
The 3rd step: be 95min cooling time, temperature is 600 ℃, logical argon gas, ingot furnace cavity pressure is 710mbar;
The 4th step: be 365min cooling time, temperature is 410 ℃, logical argon gas, ingot furnace cavity pressure is 710 mbar;
The 5th step: be 25min cooling time, temperature is 390 ℃, logical argon gas, ingot furnace cavity pressure is 860mbar;
After cooling the completing of above-mentioned 5 steps, ingot furnace cavity temperature is during lower than 400 ℃, when applying argon gas in stove reaches 980mbar, can open ingot furnace; With dummy car, inserting with the crucible of ingot casting, out deliver to indoor regulation place and naturally cool to room temp, the square ingot of pulling down after crucible 1 meter of square height and be 325 centimetres has been made into, and carries out evolution, flour milling, section and finally makes cell piece.
Embodiment tri-: a kind of manufacture craft of efficient fritting polycrystalline cast ingot, comprises the following steps:
(1) raw material: primary polysilicon 65%, polycrystalline auxiliary material 35%; Polycrystalline auxiliary material is one or more in broken polycrystalline, polycrystalline flaw-piece, polycrystal tail, monocrystalline tailing, polycrystalline head material;
(2) raw material is encased in crucible, crucible is sent in ingot furnace, be positioned on DS piece (heat exchange mass);
(3) heat-processed comprises following 5 steps:
The 1st step: be 12min heat-up time, Heating temperature is 160 ℃, vacuum tightness is 0.01mbar;
The 2nd step: be 35min heat-up time, Heating temperature is 420 ℃, vacuum tightness is 0.01mbar;
The 3rd step: be 95min heat-up time, Heating temperature is 750 ℃, vacuum tightness is 0.01mbar;
The 4th step: be 125min heat-up time, Heating temperature is 1150 ℃, vacuum tightness is 0.01mbar;
The 5th step: be 152min heat-up time, Heating temperature is 1172 ℃, vacuum tightness is 0.01mbar;
(4) melting process comprises following 13 steps:
The 1st step: be 32min heat-up time, Heating temperature is 1176 ℃, ingot furnace cavity pressure set(ting)value is 0.01mbar;
The 2nd step: be 13min heat-up time, Heating temperature is 1194 ℃, logical argon gas, ingot furnace cavity pressure is 194mbar;
The 3rd step: be 13min heat-up time, Heating temperature is 1214 ℃, logical argon gas, ingot furnace cavity pressure 354mbar;
The 4th step: be 184min heat-up time, Heating temperature is 1456 ℃, logical argon gas, ingot furnace cavity pressure is 503 mbar;
The 5th step: be 92min heat-up time, Heating temperature is 1502 ℃, logical argon gas, ingot furnace cavity pressure is 552 mbar;
The 6th step: be 241min heat-up time, Heating temperature is 1541 ℃, logical argon gas, ingot furnace cavity pressure is 551mbar;
The 7th step: be 721min heat-up time, Heating temperature is 1539 ℃, logical argon gas, ingot furnace cavity pressure is 551mbar, upper is 0.7cm every cage valve lift;
The 8th step: be 34min heat-up time, Heating temperature is 1534 ℃, logical argon gas, ingot furnace cavity pressure is 554mbar, upper every cage valve lift maintenance 0.7cm; ;
The 9th step: be 34min heat-up time, Heating temperature is 1484 ℃, logical argon gas, ingot furnace cavity pressure is 554 mbar, upper every cage valve lift maintenance 0.7cm;
The 10th step: be 94min heat-up time, Heating temperature is 1446 ℃, logical argon gas, ingot furnace cavity pressure is 554 mbar, upper every cage valve lift maintenance 0.7cm;
The 11st step: be 16min heat-up time, Heating temperature is 1446 ℃, logical argon gas, ingot furnace cavity pressure is 554mbar, upper is 7cm every cage valve lift;
(5) grow brilliant process and comprise following 9 steps:
The 1st step: be 184min heat-up time, Heating temperature is 1446 ℃, logical argon gas, ingot furnace cavity pressure is 554mbar;
The 2nd step: be 181min heat-up time, Heating temperature is 1443 ℃, logical argon gas, ingot furnace cavity pressure is 551 mbar;
The 3rd step: be 62min heat-up time, Heating temperature is 1442 ℃, logical argon gas, ingot furnace cavity pressure is 554mbar;
The 4th step: be 304min heat-up time, Heating temperature is 1436 ℃, logical argon gas, ingot furnace cavity pressure is 554mbar;
The 5th step: be 484min heat-up time, Heating temperature is 1424 ℃, logical argon gas, ingot furnace cavity pressure is 554 mbar;
The 6th step: be 244min heat-up time, Heating temperature is 1422 ℃, logical argon gas, ingot furnace cavity pressure is 5534mbar;
The 7th step: heat-up time 484min, Heating temperature is 1420 ℃, logical argon gas, ingot furnace cavity pressure is 554mbar;
The 8th step: be 214min heat-up time, Heating temperature is 1419 ℃, logical argon gas, ingot furnace cavity pressure is 554mbar;
(6) annealing process: be 226min heat-up time, Heating temperature is 1370 ℃, logical argon gas, ingot furnace cavity pressure is 604 mbar;
(7) coolingly comprise following 5 steps:
The 1st step: be 184min cooling time, temperature is 1200 ℃, logical argon gas, ingot furnace cavity pressure is 605mbar;
The 2nd step: be 184min cooling time, temperature is 1000 ℃, logical argon gas, ingot furnace cavity pressure is 605mbar;
The 3rd step: be 94min cooling time, temperature is 700 ℃, logical argon gas, ingot furnace cavity pressure is 705mbar;
The 4th step: be 364min cooling time, temperature is 500 ℃, logical argon gas, ingot furnace cavity pressure is 705 mbar;
The 5th step: be 24min cooling time, temperature is 400 ℃, logical argon gas, ingot furnace cavity pressure is 855mbar;
After cooling the completing of above-mentioned 5 steps, ingot furnace cavity temperature is during lower than 400 ℃, when applying argon gas in stove reaches 980mbar, can open ingot furnace; With dummy car, inserting with the crucible of ingot casting, out deliver to indoor regulation place and naturally cool to room temp, the square ingot of pulling down after crucible 1 meter of square height and be 325 centimetres has been made into, and carries out evolution, flour milling, section and finally makes cell piece.
By test, the polycrystalline cast ingot efficiency of conversion that the manufacture craft of efficient fritting polycrystalline cast ingot of the present invention obtains reaches 17.6%; Bottom polycrystalline crystalline substance is spent evenly, and dislocation is few, and lattice defect is few.
Claims (3)
1. a manufacture craft for efficient fritting polycrystalline cast ingot, is characterized in that, comprises the following steps:
(1) raw material: primary polysilicon 60～70%, polycrystalline auxiliary material 30～40%;
(2) raw material is encased in crucible, crucible is sent in ingot furnace, be positioned on DS piece; Crucible is positioned on DS piece, and crucible upper cover is established well heater, and well heater outside is upper heat-insulation cage, and DS piece bottom is lower thermal insulation layer;
(3) heat-processed comprises following 5 steps:
The 1st step: be 10～15min heat-up time, Heating temperature is 150～200 ℃, vacuum tightness is 0.02～0.006mbar;
The 2nd step: be 30～40min heat-up time, Heating temperature is 400～450 ℃, vacuum tightness is 0.02～0.006mbar;
The 3rd step: be 90～100min heat-up time, Heating temperature is 700～800 ℃, vacuum tightness is 0.02～0.006mbar;
The 4th step: be 120～130min heat-up time, Heating temperature is 1100～1175 ℃, vacuum tightness is 0.02～0.006mbar;
The 5th step: be 150～155min heat-up time, Heating temperature is 1170～1175 ℃, vacuum tightness is 0.02～0.006mbar;
(4) melting process comprises following 13 steps:
The 1st step: be 30～35min heat-up time, Heating temperature is 1175～1180 ℃, ingot furnace cavity pressure set(ting)value is 0.02～0.006 mbar;
The 2nd step: be 12～15min heat-up time, Heating temperature is 1193～1195 ℃, logical argon gas, ingot furnace cavity pressure is 190～195 mbar;
The 3rd step: be 12～15min heat-up time, Heating temperature is 1210～1215 ℃, logical argon gas, ingot furnace cavity pressure 350～355mbar;
The 4th step: be 180～185min heat-up time, Heating temperature is 1455～1460 ℃, logical argon gas, ingot furnace cavity pressure is 500～505 mbar;
The 5th step: be 90～95min heat-up time, Heating temperature is 1500～1505 ℃, logical argon gas, ingot furnace cavity pressure is 550～555 mbar;
The 6th step: be 240～245min heat-up time, Heating temperature is 1540～1545 ℃, logical argon gas, ingot furnace cavity pressure is 550～555mbar;
The 7th step: be 720～725min heat-up time, Heating temperature is 1538～1540 ℃, logical argon gas, ingot furnace cavity pressure is 550～555 mbar, upper is 0.6～0.8cm every cage valve lift;
The 8th step: be 30～35min heat-up time, Heating temperature is 1532～1535 ℃, logical argon gas, ingot furnace cavity pressure is 550～555 mbar, upper every cage valve lift maintenance 0.6～0.8cm; ;
The 9th step: be 30～35min heat-up time, Heating temperature is 1480～1485 ℃, logical argon gas, ingot furnace cavity pressure is 550～555 mbar, upper every cage valve lift maintenance 0.6～0.8cm;
The 10th step: be 90～95min heat-up time, Heating temperature is 1445～1448 ℃, logical argon gas, ingot furnace cavity pressure is 550～555 mbar, upper every cage valve lift maintenance 0.6～0.8cm;
The 11st step: be 15～18min heat-up time, Heating temperature is 1445～1448 ℃, logical argon gas, ingot furnace cavity pressure is 550～555 mbar, upper is 6～8cm every cage valve lift;
(5) grow brilliant process and comprise following 9 steps:
The 1st step: be 180～185min heat-up time, Heating temperature is 1445～1448 ℃, logical argon gas, ingot furnace cavity pressure is 550～555mbar;
The 2nd step: be 180～182min heat-up time, Heating temperature is 1443～1444 ℃, logical argon gas, ingot furnace cavity pressure is 550～555 mbar;
The 3rd step: be 60～65min heat-up time, Heating temperature is 1442～1443 ℃, logical argon gas, ingot furnace cavity pressure is 550～555mbar;
The 4th step: be 300～305min heat-up time, Heating temperature is 1435～1438 ℃, logical argon gas, ingot furnace cavity pressure is 550～555 mbar;
The 5th step: be 480～485min heat-up time, Heating temperature is 1424～1425 ℃, logical argon gas, ingot furnace cavity pressure is 550～555 mbar;
The 6th step: be 240～245min heat-up time, Heating temperature is 1421～1423 ℃, logical argon gas, ingot furnace cavity pressure is 550～555mbar;
The 7th step: heat-up time 480～485min, Heating temperature is 1419～1421 ℃, logical argon gas, ingot furnace cavity pressure is 550～555mbar;
The 8th step: be 210～215min heat-up time, Heating temperature is 1418～1420 ℃, logical argon gas, ingot furnace cavity pressure is 550～555 mbar;
(6) annealing process: be 225～230min heat-up time, Heating temperature is 1370 ℃, logical argon gas, ingot furnace cavity pressure is 600～605 mbar;
(7) coolingly comprise following 5 steps:
The 1st step: be 180～185min cooling time, temperature is 1100～1370 ℃, logical argon gas, ingot furnace cavity pressure is 600～610mbar;
The 2nd step: be 180～185min cooling time, temperature is 800～1100 ℃, logical argon gas, ingot furnace cavity pressure is 600～610mbar;
The 3rd step: be 90～95min cooling time, temperature is 600～800 ℃, logical argon gas, ingot furnace cavity pressure is 700～710mbar;
The 4th step: be 360～365min cooling time, temperature is 410～600 ℃, logical argon gas, ingot furnace cavity pressure is 700～710 mbar;
The 5th step: be 20～25min cooling time, temperature is 390～410 ℃, logical argon gas, ingot furnace cavity pressure is 850～860mbar;
After upper cooling completing, ingot furnace cavity temperature is during lower than 400 ℃, when applying argon gas in stove reaches 980mbar, can open ingot furnace, obtains polycrystalline cast ingot.
2. the manufacture craft of efficient fritting polycrystalline cast ingot as claimed in claim 1, is characterized in that: described polycrystalline auxiliary material is one or more in broken polycrystalline, polycrystalline flaw-piece, polycrystal tail, monocrystalline tailing, polycrystalline head material.
3. the manufacture craft of efficient fritting polycrystalline cast ingot as claimed in claim 1, is characterized in that: described DS piece is all around around 4.5cm thickness insulation quilt.
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| CN109208072A (en) * | 2018-05-31 | 2019-01-15 | 扬州续笙新能源科技有限公司 | A kind of method for crystallising improving polycrystalline silicon ingot casting bottom crystalline substance flower |
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