CN101864594A - Ingot casting method for quasi-monocrystalline silicon - Google Patents
Ingot casting method for quasi-monocrystalline silicon Download PDFInfo
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Abstract
The invention relates to an ingot casting method for quasi-monocrystalline silicon, which comprises the following steps of: (1) laying seed crystals at the bottom of a quartz crucible and adding a silicon material and a doping agent on the seed crystals; (2) vacuumizing and heating the crucible with the materials, raising the temperature in sections to melt the silicon material on the upper part, when the seed crystals begin to melt at the later stage of melting, controlling the temperatures and heating rates of a heater and the bottom of the crucible to partially melt the seed crystals and then entering a crystal growing stage; (3) cooling the heater in sections at the stage of crystal growing to make silicon crystals grow along the direction of unmelted seed crystals, and annealing and cooling after the silicon crystals grows to obtain large-gain silicon ingots; and (4) performing subsequent treatment on the large-grain silicon ingots to obtain the quasi-monocrystalline silicon. In the method, melting and crystal growing and the like are finished in the same equipment and in the same crucible, and the seed crystals are melted by controlling the temperature of the bottom of the crucible and the heating rate of the heater, so that the method has the advantages of low cost, easy operation and suitability for mass production; and the prepared quasi-monocrystalline silicon has high conversion efficiency, and the seed crystals can be recycled.
Description
Technical field
The invention belongs to area of solar cell, be specifically related to a kind of casting ingot method of accurate monomer silicon.
Background technology
In the photovoltaic industry of fast development, high-level efficiency and low cost are two main competition spots always, and crystalline silicon is as current topmost solar cell material, and the efficient stable that relies on its battery is always in occupation of absolute advantage.
Silicon single crystal generally adopts vertical pulling method (CZ method) to make, single crystal seed with particular crystal orientation is carried out seeding, obtain the silicon single crystal rod in target crystal orientation through rotary pulling, products obtained therefrom only contains a crystal grain, have characteristics such as low defective, high conversion efficiency, particularly the widespread use of alkali etching method makes the monocrystalline silicon battery sheet have more advantage, and the pyramid textured surfaces that this method forms has been strengthened the absorption of light greatly, has improved efficiency of conversion.At present, the efficiency of conversion of monocrystalline silicon battery sheet scale operation has reached 18%.But this method is to raw material and operational requirement height, and single feeds intake fewly, and product cost is higher.For the boron-doping monocrystalline, because the introducing of O in the monocrystalline crucible makes that the monocrystalline solar cells decay is bigger.
Polysilicon mainly is to adopt directional solidification process to make, the single charging capacity is big, have characteristics such as easy to operate, low adult, and the quartz crucible inner surface silicon nitride coating has buffer action, the silicon ingot O content of gained is relatively low, and battery sheet attenuation ratio monocrystalline silicon piece is little a lot; But under traditional ingot casting condition, a large amount of forming core points can appear after the crucible bottom cooling, be difficult to obtain super large crystal grain, so in the ingot casting polycrystalline, often contain a large amount of crystal boundaries and defective, and owing to differ in each crystal grain crystal orientation, can not adopt anisotropic alkali etching method to carry out surface treatment, isotropic sour making herbs into wool mode then is difficult to the effect that reaches same, makes the efficiency of conversion of polysilicon solar cell than monocrystalline silicon battery approximately low 1.5～2%.
So it is an effective way that improves product competitiveness that the advantage of existing silicon single crystal and polysilicon in the market is combined.More work has been done around this theme by the BP SOLAR company of the U.S., its patent US2007/0169684A1 has reported several different methods, it is that seed crystal and silicon material is placed apart that a kind of method is wherein arranged, molten silicon liquid is poured into long crystalline substance in the container that is covered with seed crystal, owing to separate two containers, process is comparatively complicated, not easy to operate; In addition, Chinese patent application 200910152970.2 has also been announced the preparation method of similarly big crystal grain casting polycrystalline silicon, but its with the monocrystalline of a certain particular crystal orientation completely as seed crystal, increased the ingot casting cost, be not suitable for scale operation.
Summary of the invention
The object of the present invention is to provide a kind of casting ingot method of silicon single crystal, all processes such as this method will melt, long crystalline substance are finished in the same crucible of same equipment, by crucible bottom temperature and the fusing of well heater temperature rise rate control seed crystal, low, the easy handling of this method cost is fit to large-scale production; The silicon single crystal efficiency of conversion height of preparation, and can be used as the seed crystal recycling.
For achieving the above object, the casting ingot method of silicon single crystal provided by the invention comprises following steps:
(1) chooses seed crystal and be laid on the quartz crucible bottom, on seed crystal, add the silicon material, and add doping agent according to target resistivity;
(2) crucible that above-mentioned raw materials will be housed places ingot furnace to vacuumize and heats, temperature-gradient method makes the silicon material fusing on top, to melting the later stage, when seed crystal begins to melt, the temperature rise rate of control heater temperature, crucible bottom temperature and crucible bottom, make the seed crystal partial melting, enter the long brilliant stage then;
(3) in the long brilliant stage, with heater temperature segmentation cooling, make silicon crystal along unfused seed crystal direction stable growth, treat that silicon crystal grows up to after, obtain big crystal grain silicon ingot through annealing, cooling;
(4) big crystal grain silicon ingot is obtained being used to make the quasi-monocrystalline silicon of solar cell through subsequent disposal.
In above-mentioned steps:
At least one face of seed crystal described in the step (1) is smooth, can stablize with the quartz crucible inner bottom surface to contact.
Seed crystal described in the step (1) can also be the single crystal ingot close or identical with the target crystal state or the polycrystalline piece more than one or that can splice mutually.
Seed crystal described in the step (1) can also be for the polysilicon behind the evolution little side's ingot through blocking the polysilicon block made or the single crystal rod behind the evolution through blocking the monocrystalline silico briquette of making, its thickness is 5～50mm.
Seed crystal described in the step (1) can also be the polysilicon block in main crystal orientation for the single crystal ingot in (100) crystal orientation or with (100).
When seed crystal begins to melt in the step (2), the control heater temperature is 1410～1600 ℃, regulating the crucible bottom temperature simultaneously is 1200～1410 ℃, and the crucible bottom temperature rise rate is 0.01～0.5 ℃/min, make the seed crystal partial melting, and enter the long brilliant stage according to seed crystal desired height end fusing.
The process of the segmentation cooling described in the step (3) is: heater temperature is reduced to 1410～1500 ℃ earlier fast, simultaneously heat-insulation cage or thermal baffle are opened with selected speed, the bottom heat radiation realizes directional freeze, after treating that interface growth steadily, continue the segmentation cooling again, and open heat-insulation cage or thermal baffle with selected speed, make silicon crystal along unfused seed crystal direction stable growth.
Subsequent disposal in the step (4) contains following operation: evolution, tail, grinding, chamfering and section detect, decaptitate.
Above-mentionedly handle that the silico briquette of back gained is selected, can be used as seed crystal after the cleaning and utilize again through the tail of decaptitating.
The chip area in a certain crystal orientation accounts for more than 50% of whole silicon wafer area in the described quasi-monocrystalline silicon of step (4).
The concrete technical process of the casting ingot method of above-mentioned quasi-monocrystalline silicon provided by the invention as shown in Figure 1.
The invention has the beneficial effects as follows: utilize the quasi-monocrystalline silicon of the super large of ingot casting technology growth cheaply crystal grain, gained battery sheet has characteristics such as low cost, high-level efficiency; Can select seed crystal flexibly according to different needs, and clout can be used as seed crystal recycling, whole technology is in tradition or improve in the ingot furnace and carry out, and is easy to operate, is easier to realize industrialization.
Description of drawings
Fig. 1 is a process flow sheet of the present invention;
Fig. 2 a and Fig. 2 b are the charging method figure of seed crystal among the embodiment 1;
Fig. 3 a and Fig. 3 b are the long brilliant process design sketchs of single crystal seed seeding among the embodiment 1;
Fig. 4 a and Fig. 4 b are the shape appearance figures of the accurate single-chip that the single crystal seed seeding obtains among the embodiment 3.
Embodiment
Embodiment 1
(100) crystal orientation single crystal rod that vertical pulling method obtains is carried out evolution, obtain the square column that cross dimensions is 156 * 156mm, be cut into the thick bulk of 40～50mm as seed crystal.The 450kg type quartz crucible of choice criteria, be that interior dimensions is 840 * 840 * 400mm, according to 25 156 * 156mm seed crystals of above Standard Selection, closely be tiled in crucible bottom by 5 * 5 modes, make seed crystal placed in the middle during placement, promptly the edge identity distance crucible inwall size of peripheral seed crystal is close as far as possible.Place primary polycrystalline above the seed crystal again, comprise the seed crystal 430kg that feeds altogether, the filling mode of the concrete arrangement mode of seed crystal and seed crystal, silicon material and doping agent is shown in accompanying drawing 2a, 2b, and doping agent is boron, sows or phosphorus that the back target crystalline resistivity of mixing is 1.50～2.0 Ω .cm.
Place ingot furnace to vacuumize in the crucible that above-mentioned raw materials is housed and heat, ingot furnace is traditional ingot furnace or the JJL500 type ingot furnace after improved ingot furnace such as thermal field improve etc., and control power is heated to 1000～1400 ℃; After entering the fusion stage, adopt temperature control segmentation to heat, to the fusing final step well heater controlled temperature is adjusted to 1550 ℃, be retained to the seed crystal fusion stage, treat 1280 ℃ of crucible bottom temperature, and adjust temperature rise rate and up and down the time, finish the fusing step, jump to the long brilliant stage at 0.3 ℃/min.Enter the long brilliant stage, fast temperature is reduced to 1500 ℃ by 1550 ℃, in the 30min thermal baffle is opened to 10cm subsequently, bottom heat radiation realizes directional freeze, treat that interface growth steadily after, segmentation cools the temperature to 1416 ℃ again, the thermal baffle opening speed is successively opened by the speed of 1.5cm/h, 0.8cm/h, until maximum, reach stable long brilliant, long brilliant effect and long brilliant process are shown in accompanying drawing 3a and accompanying drawing 3b.
With the silicon crystal after above-mentioned growing up to, through annealing, cooling obtains big crystal grain silicon ingot, gained silicon ingot evolution gets 25 little side's ingots, can be observed from the bottom and not melt seed crystal completely, seed crystal remains about 30～35mm, the subsequent growth crystal seed crystal of postponing is upwards long, bottom 5cm is following to be monocrystalline entirely, single grain begins division afterwards, little ingot middle part still keeps big crystal grain, to then changing little crystal grain more than the 20cm into, again after testing with little side's ingot behind the evolution, the tail of decaptitating, operations such as section get monocrystalline silicon piece, (chip area in (100) crystal orientation accounts for more than 50% of the silicon chip total area in the silicon chip) ratio of accurate single-chip is 68%, and wherein 15% silicon chip is super large crystal grain sheet (chip area in (100) crystal orientation accounts for more than 90% of the silicon chip total area in the silicon chip).Behind the silicon ingot evolution, the part of the tail of decaptitating can be used as the seed crystal recycling.
Embodiment 2
(100) crystal orientation single crystal rod that vertical pulling method obtains is carried out evolution, and the silicon rod that to obtain cross dimensions be 156 * 156mm, be about 160mm and 310mm radially cuts off then, obtains being of a size of the seed crystal of 156 * 310 * 30mm, 156 * 160 * 30mm.Join with the 156mm limit by the monocrystalline silico briquette of 2 310mm of every row, 1 160mm specification and closely to arrange, divide 5 row to tile 15 seed crystals altogether in the quartz crucible of 840 * 840 * 400mm, make seed crystal placed in the middle during placement, promptly the edge identity distance crucible inwall size of peripheral seed crystal is close as far as possible.Place primary polycrystalline above the seed crystal again, comprise the seed crystal 430kg that feeds altogether, the doping target resistivity is 1.5 Ω .cm.
Vacuumize after the charging, control power is heated to 1000～1400 ℃; After entering the fusion stage, adopt temperature control segmentation to heat, the well heater controlled temperature is adjusted to 1550 ℃ to the fusing final step, be retained to the seed crystal fusion stage, treat that the crucible bottom temperature is 1375 ℃, and temperature rise rate is that 0.04 ℃/min is up and down the time, finish the fusing step, jump to the long brilliant stage.Enter the long brilliant stage, fast temperature is reduced to 1430 ℃ by 1550 ℃, closed heat insulation maintenance 30min, thermal baffle is opened to 6cm in the 1h subsequently, the bottom heat radiation realizes directional freeze, treat that interface growth steadily after, segmentation is fallen 1412 ℃ with temperature again, the thermal baffle opening speed is successively opened by the speed of 0.7cm/h, 1.4cm/h, until maximum, reaches stable long brilliant.
With the silicon crystal after above-mentioned growing up to, obtain big crystal grain silicon ingot through annealing, cooling, gained silicon ingot evolution gets 25 little side's ingots, can be observed from the bottom and not melt seed crystal completely, seed crystal remains about 5～10mm, the subsequent growth crystal seed crystal of postponing is upwards long, observe from the side, bottom 10cm is following to be monocrystalline, single grain begins division afterwards, and little ingot middle part still keeps big crystal grain, until the 20cm place, change less crystal grain into, again with little side's ingot behind the evolution after testing, operation such as the tail of decaptitating, section gets monocrystalline silicon piece.80% monocrystalline silicon piece (chip area in same crystal orientation accounts for more than 50% of the silicon chip total area in the silicon chip) that is as the criterion in the gained silicon chip, wherein 30% is super large crystal grain sheet (chip area in same crystal orientation accounts for more than 90% of the silicon chip total area in the silicon chip).Behind the silicon ingot evolution, the part of the tail of decaptitating can be used as the seed crystal recycling.
Embodiment 3
Method as embodiment 1 obtains 13 of (100) crystal orientation single crystal seed; In addition, the silicon ingot that quasi-monocrystalline silicon ingot casting is before obtained carries out evolution, detection, band saw to cut off, the bottom silico briquette (be mainly residue seed crystal) and the big crystal grain silico briquette in top of excision are selected and are processed, clean after removing impurity enriched layer up and down, with it as another part seed crystal.The bottom residue seed crystal silico briquette, the big crystal grain silico briquette in top that reclaim in this example are respectively got 6 as seed crystal, thickness 2.5～3cm.25 seed crystals that more than obtain are closely arranged by 5 * 5 mode and are tiled in the standard quartz crucible that interior dimensions is 840 * 840 * 400mm, arrange to make effect comparison by different sorts seed crystal symmetrical manner during arrangement.Contain seed crystal at the interior 430kg that feeds altogether, and according to target resistivity 1.5 Ω .cm add doping agent.
Vacuumize after the charging, control power heats; After entering the fusion stage, adopt temperature control segmentation to heat, to the fusing final step well heater controlled temperature is adjusted to 1540 ℃, be retained to the seed crystal fusion stage, treat that the crucible bottom temperature is 1350 ℃, and the bottom temperature rise rate is 0.07 ℃/min up and down the time, finishes the fusing step, jumps to the long brilliant stage.Enter the long brilliant stage, fast temperature is reduced to 1440 ℃ by 1540 ℃, and close thermal baffle (cage) and keep 1h, afterwards thermal baffle (cage) is opened 5cm fast, bottom heat radiation realizes directional freeze, treat that interface growth steadily after, segmentation is fallen 1415 ℃ with temperature again, thermal baffle (cage) opening speed successively opens to 20cm by the speed of 0.5cm/h, 0.7cm/h, reaches stable long brilliant.
With the silicon crystal after above-mentioned growing up to, obtain silicon ingot through annealing, cooling, gained silicon ingot evolution gets 25 little side's ingots, and the seed crystal that makes discovery from observation remains about 15～20mm and does not melt, the crystal continued growth on the seed crystal direction of postponing.Big crystal grain runs through whole silicon ingot to the top by the bottom in the silicon ingot, the big crystal grain of upper surface (＞50mm) area is greater than 50%, and the shape appearance figure of the quasi-monocrystalline silicon sheet that the little side's ingot of single crystal seed prepares is shown in accompanying drawing 4a, 4b.Contrast the brilliant effect of length of three seed crystal block correspondences: the continuity single crystal growing of single crystal seed place, to occurring a small amount of division crystal grain more than the 10cm, big crystal grain extends to the silicon ingot top, and little ingot is cut into slices between 380～470,95% monocrystalline silicon piece that is as the criterion, wherein super large crystal grain silicon chip accounts for 35～60%; The bottom residue seed crystal seeding of recycling and the brilliant effect of follow-up length and single crystal seed do not have too big difference; The big grain growing of the same continuity of the big crystal grain seed crystal of recycling in top, little ingot gained silicon chip 70～90% single-chip that is as the criterion, wherein 15～34% is super large crystal grain silicon chip.The ensemble average minority carrier life time of each little side's ingot is all greater than 4 μ s, and 2 μ s detect line by minority carrier life time, silicon ingot yield 62.7%.The battery sheet efficiency of conversion 17.9% that the gained monocrystalline silicon piece is made is suitable with the conventional monocrystalline silicon piece of same production line.
The specific embodiment of more than enumerating is the explanation that the present invention is carried out.It is pointed out that above embodiment only is used for that the invention will be further described, do not represent protection scope of the present invention, nonessential modification and adjustment that other people prompting according to the present invention is made still belong to protection scope of the present invention.
Claims (10)
1. the casting ingot method of a quasi-monocrystalline silicon is characterized in that: comprise following steps:
(1) chooses seed crystal and be laid on the quartz crucible bottom, on seed crystal, add the silicon material, and add doping agent according to target resistivity;
(2) crucible that above-mentioned raw materials will be housed places ingot furnace to vacuumize and heats, temperature-gradient method makes the silicon material fusing on top, to melting the later stage, when seed crystal begins to melt, the temperature rise rate of control heater temperature, crucible bottom temperature and crucible bottom, make the seed crystal partial melting, enter the long brilliant stage then;
(3) in the long brilliant stage, with heater temperature segmentation cooling, make silicon crystal along unfused seed crystal direction stable growth, treat that silicon crystal grows up to after, obtain big crystal grain silicon ingot through annealing, cooling;
(4) big crystal grain silicon ingot is obtained being used to make the quasi-monocrystalline silicon of solar cell through subsequent disposal.
2. the casting ingot method of quasi-monocrystalline silicon according to claim 1, it is characterized in that: at least one face of seed crystal described in the step (1) is smooth, can stablize with the quartz crucible inner bottom surface to contact.
3. the casting ingot method of quasi-monocrystalline silicon according to claim 1 is characterized in that: with target crystal state close or identical single crystal ingot or the polycrystalline piece one piece or one piece or more of the seed crystal described in the step (1) for splicing mutually.
4. the casting ingot method of quasi-monocrystalline silicon according to claim 1, it is characterized in that: the seed crystal described in the step (1) is the little side's ingot of the polysilicon behind the evolution through blocking the polysilicon block made or the single crystal rod behind the evolution through blocking the monocrystalline silico briquette of making, and its thickness is 5～50mm.
5. the casting ingot method of quasi-monocrystalline silicon according to claim 1 is characterized in that: the seed crystal described in the step (1) is the polysilicon block in main crystal orientation for the single crystal ingot in (100) crystal orientation or with (100).
6. the casting ingot method of quasi-monocrystalline silicon according to claim 1, it is characterized in that: when seed crystal begins to melt in the step (2), the control heater temperature is 1410～1600 ℃, regulating the crucible bottom temperature simultaneously is 1200～1410 ℃, and the crucible bottom temperature rise rate is 0.01～0.5 ℃/min, make the seed crystal partial melting, and enter the long brilliant stage according to seed crystal desired height end fusing.
7. the casting ingot method of quasi-monocrystalline silicon according to claim 1, it is characterized in that: the process of the segmentation cooling described in the step (3) is: heater temperature is reduced to 1410～1500 ℃ earlier fast, simultaneously heat-insulation cage or thermal baffle are opened with selected speed, the bottom heat radiation realizes directional freeze, after treating that interface growth steadily, continue the segmentation cooling again, and open heat-insulation cage or thermal baffle, make silicon crystal along unfused seed crystal direction stable growth with selected speed.
8. the casting ingot method of quasi-monocrystalline silicon according to claim 1, it is characterized in that: the subsequent disposal in the step (4) contains following operation: evolution, tail, grinding, chamfering and section detect, decaptitate.
9. the casting ingot method of quasi-monocrystalline silicon according to claim 8 is characterized in that: handle that the silico briquette of back gained is selected, can be used as seed crystal after the cleaning and utilize again through the tail of decaptitating.
10. the casting ingot method of quasi-monocrystalline silicon according to claim 1, it is characterized in that: the chip area in a certain crystal orientation accounts for more than 50% of whole silicon wafer area in the described quasi-monocrystalline silicon of step (4).
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