CN102797036B - Polycrystal silicon ingot and manufacture method, solaode - Google Patents
Polycrystal silicon ingot and manufacture method, solaode Download PDFInfo
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- CN102797036B CN102797036B CN201210017967.1A CN201210017967A CN102797036B CN 102797036 B CN102797036 B CN 102797036B CN 201210017967 A CN201210017967 A CN 201210017967A CN 102797036 B CN102797036 B CN 102797036B
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 195
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 195
- 239000010703 silicon Substances 0.000 title claims abstract description 195
- 238000000034 method Methods 0.000 title claims abstract description 88
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 34
- 239000013078 crystal Substances 0.000 claims abstract description 135
- 238000002425 crystallisation Methods 0.000 claims abstract description 52
- 230000008025 crystallization Effects 0.000 claims abstract description 47
- 239000007788 liquid Substances 0.000 claims abstract description 46
- 239000007787 solid Substances 0.000 claims abstract description 38
- 239000002994 raw material Substances 0.000 claims abstract description 35
- 239000000155 melt Substances 0.000 claims abstract description 6
- 229910021421 monocrystalline silicon Inorganic materials 0.000 claims description 28
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 11
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 9
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 9
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 9
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 3
- 239000012535 impurity Substances 0.000 abstract description 41
- 230000009466 transformation Effects 0.000 abstract description 11
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 22
- 229920005591 polysilicon Polymers 0.000 description 18
- 230000007547 defect Effects 0.000 description 17
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 16
- 239000001301 oxygen Substances 0.000 description 16
- 229910052760 oxygen Inorganic materials 0.000 description 16
- 238000005266 casting Methods 0.000 description 13
- 238000009833 condensation Methods 0.000 description 7
- 230000005494 condensation Effects 0.000 description 7
- 239000000047 product Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 239000004484 Briquette Substances 0.000 description 3
- XGCTUKUCGUNZDN-UHFFFAOYSA-N [B].O=O Chemical compound [B].O=O XGCTUKUCGUNZDN-UHFFFAOYSA-N 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000000977 initiatory effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 1
- 239000006117 anti-reflective coating Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 210000000746 body region Anatomy 0.000 description 1
- 239000002800 charge carrier Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 150000003376 silicon Chemical class 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
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- Silicon Compounds (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Photovoltaic Devices (AREA)
Abstract
The invention discloses the manufacture method of a kind of polycrystal silicon ingot, including: the container bottom in polycrystal silicon ingot growth furnace lays seed crystal, forms inculating crystal layer; The silicon raw material of solid-state is loaded into the top of inculating crystal layer; Described container being heated, melts described silicon raw material and the described inculating crystal layer of part, form liquid level, at least keeping the part inculating crystal layer contacted with container bottom is solid-state; Control the thermal field in polycrystal silicon ingot growth furnace, liquid level is carried out crystallization and forms crystallizing layer, so that solid liquid interface moves to the direction away from described container bottom; After solid liquid interface moves respective distance to the direction away from described container bottom, enter melt back crystallization process, after at least performing once described melt back crystallization process, obtain polycrystal silicon ingot. Adopting the polycrystal silicon ingot impurity content that the method for the present invention is produced low, the solaode cost produced is low, attenuation quotient is low, and photoelectric transformation efficiency is high.
Description
Technical field
The present invention relates to monocrystal silicon, the manufacturing technology of polysilicon and photoelectric field, particularly relate to a kind of polycrystal silicon ingot and manufacture method, solaode.
Background technology
Solaode can convert light energy into electric energy, and the height of photoelectric transformation efficiency and the speed of cell decay are the important parameters weighing solaode quality. At present, the difference according to material, solaode is broadly divided into monocrystaline silicon solar cell and polysilicon solar cell two kinds.
Wherein, monocrystal silicon is by after the silicon raw materials melt containing adulterant, silicon metal is pulled out melt region and what crystallization was formed, the method generally producing monocrystal silicon has melt vertical pulling method (Czochralski, it is called for short CZ method) and floating zone method (being called for short FZ method), CZ method is slowly to be pulled out from melted silicon liquid by monocrystal silicon, and FZ method is and again to be solidified on the opposite side of described melt region for solid materials by melt region.
Owing to intercrystalline orientation is fixing, therefore the photoelectric transformation efficiency of monocrystaline silicon solar cell is higher, but, from production cost, adopting the monocrystal silicon single yield that both approaches produces few, and production cost is higher, especially the silicon single crystal rod of FZ method production is smaller; The performance of the silicon single crystal rod produced, silicon single crystal rod comprises radially-arranged impurity and defect, as oxygen induces ring and the space of stacking fault (OSF), or " whirlpool " defect of vacancy cluster, for CZ method, use due to silica crucible, more oxygen impurities inevitably will be comprised inside monocrystal silicon, boron oxygen (B-O) complex that oxygen impurities produces after being combined with the boron of doping is again the principal element causing solaode decay, therefore, the attenuation quotient using the solaode that this silicon single crystal rod makes is higher.
The method that polycrystal silicon ingot is typically with casting processes, and casting polysilicon is to be placed in silica crucible by melted raw silicon, and by controlling the cooling procedure of molten silicon, obtains after making molten silicon crystallization. Relative to monocrystal silicon, more defect is there is in polycrystal silicon ingot, crystal grain is little, crystal boundary and dislocation between conventional polycrystalline silicon crystal grain are more, thus causing the quick compound of electric charge carrier, cause that minority carrier life time is low, and, owing to the orientation between crystal grain is random, cause being difficult to wafer surface is carried out good texture, make conventional polycrystalline silicon solar cell lower than the photoelectric transformation efficiency of monocrystaline silicon solar cell, but the oxygen content in polycrystal silicon ingot can control in good level, so that the attenuation quotient of polysilicon solar cell is relatively low.
Summary of the invention
For solving above-mentioned technical problem, the invention provides a kind of polycrystal silicon ingot and manufacture method, solaode, relative to monocrystaline silicon solar cell of the prior art, adopt at the bottom of the cost of solaode that the polycrystal silicon ingot that the embodiment of the present invention provides produces, attenuation quotient lower, simultaneously, relative to polysilicon solar cell of the prior art, the photoelectric transformation efficiency of the solaode that the polycrystal silicon ingot that the employing embodiment of the present invention provides is produced is higher.
For solving the problems referred to above, embodiments provide following technical scheme:
A kind of manufacture method of polycrystal silicon ingot, including:
Container bottom in polycrystal silicon ingot growth furnace lays seed crystal, forms inculating crystal layer;
The silicon raw material of solid-state is loaded into the top of described inculating crystal layer;
Described container being heated, melts described silicon raw material and the described inculating crystal layer of part, to form liquid level, at least keeping the part inculating crystal layer contacted with described container bottom is solid-state;
Control the thermal field in described polycrystal silicon ingot growth furnace, described liquid level is carried out crystallization and forms crystallizing layer, so that solid liquid interface moves to the direction away from described container bottom;
After described solid liquid interface moves respective distance to the direction away from described container bottom, enter melt back crystallization process, after at least performing once described melt back crystallization process, obtain polycrystal silicon ingot;
Wherein, described melt back crystallization process includes, control the thermal field in described polycrystal silicon ingot growth furnace, described crystallizing layer is carried out melt back, described solid liquid interface is made to move to the direction near described container bottom, afterwards, control the thermal field in described polycrystal silicon ingot growth furnace, liquid level is carried out crystallization, so that described solid liquid interface moves to the direction away from described container bottom, the distance that the distance that described solid liquid interface moves to the direction near described container bottom moves to the direction away from described container bottom less than described solid liquid interface.
Preferably, described polycrystal silicon ingot contains the large-sized monocrystalline silicon region of continuous print, and the crystalline orientation of described monocrystalline silicon region is identical with the crystalline orientation of the described seed crystal being disposed below.
Preferably, the described seed crystal monocrystal silicon that to be crystalline orientation be (100), (110) or (111).
Preferably, the silicon raw material of solid-state is loaded into the process of the top of described inculating crystal layer particularly as follows:
Short grained silicon raw material is loaded into the top of described inculating crystal layer, to fill the gap between described seed crystal and the gap between described inculating crystal layer and described container side wall;
The silicon raw material of large volume is loaded into the top of described little granular silicon feedstock.
Preferably, the thickness of described inculating crystal layer is 10mm-100mm.
Preferably, when first time starts crystallization, the thickness of solid seed crystal layer is 1mm-50mm.
Preferably, the area of described inculating crystal layer occupies the 50%-99% of described container bottom area.
Preferably, described container is silica crucible, silicon carbide crucible or silicon nitride crucible.
The embodiment of the invention also discloses a kind of polycrystal silicon ingot adopting said method to make, described polycrystal silicon ingot comprises continuous large-sized monocrystalline silicon region that crystalline orientation is consistent.
The embodiment of the invention also discloses a kind of solaode, adopt above-described polycrystal silicon ingot, including:
Wafer, described wafer has continuous large-sized monocrystalline silicon region that crystalline orientation is consistent;
P-N junction in described wafer;
Conductive contact on described wafer.
Compared with prior art, technique scheme has the advantage that
The technical scheme that the embodiment of the present invention provides, the method adopting casting produces polycrystal silicon ingot, inculating crystal layer is formed by laying large area seed crystal in advance at container bottom, the growth of monocrystalline silicon region is guided by seed crystal, and by repeatedly melt back crystallization, making to comprise continuous large-sized monocrystalline silicon region in the polycrystal silicon ingot produced, the polycrystal silicon ingot namely cast out is the monocrystalline silicon region consistent with seed crystal orientation by major part, and least a portion of polysilicon region composition. Owing in casting process, the inculating crystal layer of bottom has completely cut off the oxygen of container bottom, thus the oxygen impurities content reduced in polycrystal silicon ingot, and, containing large-sized monocrystalline silicon region in polycrystal silicon ingot. Therefore, adopting the solaode that the polycrystal silicon ingot that the embodiment of the present invention provides is produced, monocrystaline silicon solar cell attenuation quotient more of the prior art is lower, and polysilicon solar cell photoelectric transformation efficiency more of the prior art is higher.
And, owing to the present embodiment adopting the mode of repeatedly melt back crystallization form polycrystal silicon ingot, slow down the setting rate of crystal to a certain extent, make impurity (such as carborundum, silicon nitride etc.) there is time enough to carry out fractional condensation, even if the impurity in raw material dissolves in the solution after can precipitating out again, thus avoiding impurity to be deposited in the crystalline region solidified, and then decrease the Hard Inclusion in cast main body and impurity enriched layer, the defect concentration in the polycrystal silicon ingot produced is made to be substantially reduced, also improve minority carrier life time to a certain extent, thus improve the photoelectric transformation efficiency of solaode.
Accompanying drawing explanation
In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, the accompanying drawing used required in embodiment or description of the prior art will be briefly described below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the premise not paying creative work, it is also possible to obtain other accompanying drawing according to these accompanying drawings
Fig. 1 is the schematic flow sheet of the manufacture method of polycrystal silicon ingot disclosed in the embodiment of the present invention one;
Fig. 2 a-Fig. 2 d is the melt back growth course schematic diagram of polycrystal silicon ingot disclosed in the embodiment of the present invention one;
Fig. 3 is the schematic flow sheet of the manufacture method of polycrystal silicon ingot disclosed in the embodiment of the present invention two;
Fig. 4 is seed crystal paving mode top view disclosed in the embodiment of the present invention two;
Fig. 5 is the disclosed profile loading silicon raw material mode of the embodiment of the present invention two;
Fig. 6 is the profile of the polycrystal silicon ingot produced in the embodiment of the present invention two.
Detailed description of the invention
Just as described in the background section, the monocrystal silicon production capacity that produces of mode adopting prior art is little, and production cost is high, and owing to oxygen impurities is more so that the attenuation quotient adopting the solaode that monocrystal silicon of the prior art makes is higher; And adopt the polycrystal silicon ingot produced in prior art, although production capacity is big, but owing to polysilicon self grain orientation is random, can not adopt chemical method that its surface is carried out good texture, thus the polysilicon surface reflectance to light can not better be reduced, improve the features such as the absorbance to light, cause that polysilicon solar cell photoelectric transformation efficiency is low.
Monocrystal silicon has the drawback that polysilicon grain orientation is random to be had the drawback that by itself structures shape, and producing same product in the same way if still adopting, these defects are exactly inevitable due to mode of production formation itself.
Additionally, polycrystal silicon ingot is except the defect of the self structure such as grain orientation is random, also has other defect caused because of technological reason, the defect such as dislocation and pit such as impurity Hard Inclusion and initiation thereof, inventor studies discovery, the reason these situations occur is, in the directional solidification process of crystal growth, owing to segregation coefficient is less, carbon in silicon raw material, the impurity such as nitrogen can be enriched with at solid liquid interface place, when speed of growth ratio is time very fast, impurity has little time fractional condensation, carborundum will be formed, silicon nitride etc., precipitate out from solution, retain in solid multi-crystalline silicon after crystallisation, become impurity enriched layer or in crystal the Hard Inclusion of pinning.
If impurity is concentrated in samdwich in cast main body, then the part silico briquette comprising impurity layer will be cut, and whole silico briquette even can be caused in some cases to scrap; If impurity precipitates out with the form of Hard Inclusion, then can become the initiating accident sequence of the defect such as dislocation and pit, cause that defect concentrations in crystals increases, Quality Down, and, owing to the hardness of carborundum, silicon nitride is all higher than silicon crystal, in section and evolution process, its higher hardness can greatly affect the quality of cutting, stria, groove is formed at cutting surfaces, even break, make whole silico briquette scrap, it is impossible to be processed as final products.
Based on above reason, inventor considers that the yield of the polycrystal silicon ingot that casting method produces is bigger, and the oxygen content of the polycrystal silicon ingot produced is relatively low, exactly solve the defect of the mode of production of monocrystal silicon, and, monocrystaline silicon solar cell is due to the reason of material, exactly there is no many defects of polysilicon solar cell, if the advantage of the two is combined, the mode producing polycrystal silicon ingot is adopted to go to produce the polycrystal silicon ingot containing large-sized monocrystalline silicon region, the shortcoming of monocrystaline silicon solar cell and polysilicon solar cell in prior art should be able to be solved to a certain extent.
Further, the method for casting is adopted to carry out in production process, it is possible to take to slow down the mode of the setting rate of crystal, reduce the Hard Inclusion in cast main body and impurity enriched layer, thus improving the quality of finished product.
It is above the core concept of the application, below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that, described embodiment is only a part of embodiment of the present invention, rather than whole embodiments. Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art obtain under not making creative work premise, broadly fall into the scope of protection of the invention.
Elaborate a lot of detail in the following description so that fully understanding the present invention, but the present invention can also adopt other to be different from alternate manner described here to be implemented, those skilled in the art can do similar popularization when without prejudice to intension of the present invention, and therefore the present invention is not by the restriction of following public specific embodiment.
Secondly, the present invention is described in detail in conjunction with schematic diagram, when describing the embodiment of the present invention in detail; for ease of explanation; representing that the profile of device architecture can be disobeyed general ratio and be made partial enlargement, and described schematic diagram is example, it should not limit the scope of protection of the invention at this. Additionally, the three-dimensional space of length, width and the degree of depth should be comprised in actual fabrication.
Embodiment one
Based on, on the basis of the studies above, embodiments providing the manufacture method of a kind of polycrystal silicon ingot, the flow chart of the method is as it is shown in figure 1, comprise the following steps:
Step S101: the container bottom in polycrystal silicon ingot growth furnace lays seed crystal, forms inculating crystal layer;
Wherein, described seed crystal is the monocrystal silicon that crystalline orientation is fixing, described inculating crystal layer includes the monocrystalline silicon layer of at least one crystalline orientation, it is preferred that the seed crystal in the present embodiment is the monocrystal silicon of (100), (110) or (111) orientation.
Concrete, in the present embodiment, inculating crystal layer includes the monocrystalline silicon layer of at least one crystalline orientation, in other words, described inculating crystal layer can all select have same crystalline orientation monocrystal silicon, as all adopted the monocrystal silicon with (100) orientation, can also partly select the monocrystal silicon with first crystal orientation, another part selects the monocrystal silicon with the second crystalline orientation, described first crystal orientation is different from described second crystalline orientation, as: a part selects the monocrystal silicon with (100) orientation, another part selects the monocrystal silicon with (110) orientation, which kind of seed crystal specifically chosen, determine according to the requirement to polycrystal silicon ingot.
The present embodiment does not specifically limit the paving mode of described inculating crystal layer, however, to ensure that the quality of the monocrystal silicon in polycrystal silicon ingot, preferably, described seed crystal is layed in the zone line of described container, additionally, in order to better control manufacturing process and the quality of described polycrystal silicon ingot, described inculating crystal layer should keep substantially parallel or less parallel with described container bottom.
Same, the present embodiment does not also specifically limit the thickness of described inculating crystal layer, determine with concrete production process and working condition, preferably, the thickness of described inculating crystal layer is 2mm-400mm, it is furthermore preferred that the thickness of described inculating crystal layer is 10mm-100mm, it is furthermore preferred that the thickness of described inculating crystal layer is 10mm-60mm.
Additionally, the container shapes in polycrystal silicon ingot growth furnace and material in the present embodiment are determined by the polycrystal silicon ingot growth furnace adopted in production process, generally, due to the present embodiment is adopt casting mode produce polycrystal silicon ingot, described container is crucible, more common for silica crucible, certainly, described container can also select other can be used for the casting process of polycrystal silicon ingot can disposable crucible or reusable crucible, such as silicon carbide crucible or silicon nitride crucible etc.
" casting " process described in the present embodiment specifically refers to for keeping in the mould of molten silicon or container by molten silicon is cooled into silicon ingot.Step S102: the silicon raw material of solid-state is loaded into the top of described inculating crystal layer;
Not limiting the mode of the silicon raw material loading described solid-state in the present embodiment, the concrete mode loading silicon raw material is determined according to the size of silicon raw material, as long as guaranteeing material to be reasonably loaded in container, and can guarantee that the safety of melt process crucible etc.
Step S103: described container is heated, melts described silicon raw material and the described inculating crystal layer of part, and to form liquid level, at least keeping the part inculating crystal layer contacted with described container bottom is solid-state;
Adopt different polycrystal silicon ingot growth furnace, the method that described container is heated also just is not quite similar, as adopted the growth furnace of heat-exchanging method, adopting the growth furnace of Bridgman method or adopt the growth furnace of the two combined technology, its heating means are had nothing in common with each other, as long as the silicon raw material of solid-state and part inculating crystal layer can be melted, meet the fusing demand of this step.
It should be noted that, this step does not limit the contact condition of solid liquid interface and container bottom, solid liquid interface can have little angle with container bottom, or solid liquid interface has a small amount of rough region, can also be parallel with container bottom, however, to ensure that the quality of the polysilicon produced, the present embodiment is preferably, container is being heated in process, keep solid liquid interface substantially parallel with described container bottom or less parallel as far as possible, unfused seed crystal can be enable to occupy whole container bottom, and unfused part inculating crystal layer can stop that the oxygen impurities from container (crucible) bottom enters in molten silicon, to reduce the content of oxygen impurities in cast main body, the boron oxygen complex formed as reduced oxygen impurities to be combined with the boron of doping, to reduce the attenuation quotient of solaode.
Step S104: control the thermal field in described polycrystal silicon ingot growth furnace, described liquid level is carried out first time crystallization and forms crystallizing layer, so that described solid liquid interface moves to the direction away from described container bottom, when in the present embodiment, first time starts crystallization, the thickness of solid seed crystal layer is 1mm-50mm, it is preferably 5mm-30mm, more preferably 20mm;
In this step molten silicon is carried out in crystallisation by cooling process, dephlegmation due to impurity, impurity (such as carborundum, silicon nitride etc.) in silicon raw material will be enriched in solid liquid interface place, and impurity content in the solid multi-crystalline silicon after crystallization is little, if but crystallization rate is too fast, the impurity such as carborundum, silicon nitride can have little time fractional condensation and remain in the polysilicon of solid-state, become impurity enriched layer or in crystal the Hard Inclusion of pinning.
In order to avoid forming impurity enriched layer and Hard Inclusion because the speed of growth is too fast in the present embodiment, can be tried one's best by the change of control crystallization temperature and control the speed of crystallization, so that crystallization rate is unlikely to too fast or excessively slow, specifically how to control to determine according to the situation of production process.
Step S105: after described solid liquid interface moves respective distance to the direction away from described container bottom, enters melt back crystallization process, after at least performing once described melt back crystallization process, obtains polycrystal silicon ingot.
Wherein, described melt back crystallization process includes, control the thermal field in described polycrystal silicon ingot growth furnace, described crystallizing layer is carried out melt back, described solid liquid interface is made to move to the direction near described container bottom, afterwards, control the thermal field in described polycrystal silicon ingot growth furnace, liquid level is carried out crystallization, so that described solid liquid interface moves to the direction away from described container bottom, the distance that the distance that described solid liquid interface moves to the direction near described container bottom moves to the direction away from described container bottom less than described solid liquid interface.
It addition, after crystal growth completes, crystal need to be cooled to uniform temperature, remove polycrystal silicon ingot from ingot furnace, afterwards that polycrystal silicon ingot is for further processing.
As described in previous step, the crystallization rate of molten silicon can affect the quality of final products, can by slowing down Hard Inclusion and the impurity enriched layer that the mode of the speed of growth reduces in product, but owing to starting the crystallization initial stage, the speed of growth of crystal is relatively difficult to control, for avoiding drawbacks described above, therefore, the present embodiment adds the melt back crystallization process in step S105.
By melt back crystallization process, namely in certain growth stage, crystal after crystallization is carried out refuse (i.e. melt back), can making to have precipitated out the impurity being deposited in solid crystals to be re-dissolved in solution, in follow-up crystallization process again, impurity continues fractional condensation again, and so forth, be equivalent to extend to a certain extent the fractional condensation time of impurity, it is to avoid impurity precipitates out and is deposited in crystal, improves the quality of crystal.
It should be noted that, the present embodiment does not limit when which kind of degree crystallization process proceed to and carries out melt back, also specifically do not limit melt back carries out crystallization again after which kind of degree, namely not limiting described solid liquid interface, move respective distance to the direction away from described container bottom be how many, and described solid liquid interface to move respective distance to the direction near described container bottom be how many, as long as ensureing every subcrystalline height height more than melt back, namely the distance that described solid liquid interface moves to the direction away from described container bottom to the distance that the direction near described container bottom is moved less than described solid liquid interface, to ensure that crystal is in growth conditions.
It addition, do not limit the time that each melt back starts in the present embodiment, also not limiting the number of each melt back and the number of times of melt back, namely the crystal growing process in the present embodiment can have multiple, below the process of crystal growth in the present embodiment is illustrated.
One when being that molten silicon crystalline growth is to certain altitude in step S104, carry out a methback process, the crystalline silicon making solid-state carries out secondary fusion, the height of fusing is less than the height of growth, when after melt back to certain altitude, carry out secondary crystallization process, make the temperature in growth furnace maintain reduced levels always, until polycrystal silicon ingot has grown, as shown in Figure 2, this process is crystallization-melt back-crystallization, until having grown, wherein, Fig. 2 a is the view before described silicon crystal crystallization, Fig. 2 b is described silicon crystal view after crystallization on the basis of Fig. 2 a, Fig. 2 c is described silicon crystal view after melt back on the basis of Fig. 2 b, Fig. 2 d is described silicon crystal view after crystallization on the basis of Fig. 2 c, Fig. 2 illustrates: silicon liquid 91, solid liquid interface 92, silicon crystal 93 and crucible bottom 94. in figure, h1, h2, h3, h4 represent the height of silicon crystal described in Fig. 2 a～Fig. 2 d respectively, then relation between the height of silicon crystal described in Fig. 2 a～Fig. 2 d is h4 > h2 > h3 > h1, two is the circulation first passing through melt back crystallization process several times, after making the growth certain altitude of crystal step, reduce in-furnace temperature always, crystal is made to continue crystallization, namely solid liquid interface is advanced all along the direction away from container bottom, until completing the growth course of polycrystal silicon ingot, this process is after multiple process, crystallization always, until having grown, three be whole crystal growth course in carry out melt back-crystallization process always, this process is for repeat crystallization-melt back-crystallization process always, until silicon ingot has grown. concrete selection is which kind of crystal growing process above-mentioned, is not specifically limited in the present embodiment, and the foundation of selection should be under ensureing the premise of quality of polycrystal silicon ingot as far as possible, saves the time of crystal growth and required energy loss.
Concrete selection is which kind of crystal growing process above-mentioned, is not specifically limited in the present embodiment, and the foundation of selection should be under ensureing the premise of quality of polycrystal silicon ingot as far as possible, saves the time of crystal growth and required energy loss.
The technical scheme that the embodiment of the present invention provides, the method adopting casting produces polycrystal silicon ingot, inculating crystal layer is formed by laying large area seed crystal in advance at container bottom, the growth of monocrystalline silicon region is guided by seed crystal, making to comprise continuous large-sized monocrystalline silicon region in the polycrystal silicon ingot produced, the crystalline orientation of described monocrystalline silicon region is identical with the crystalline orientation of the described seed crystal being disposed below.
Owing in casting process, the inculating crystal layer of bottom has completely cut off the oxygen of container bottom to diffusion in silicon raw material, thus the content of the oxygen reduced in polycrystal silicon ingot, and, owing to polycrystal silicon ingot containing large-sized monocrystalline silicon region, the chip area of crystal is big, corresponding grain boundary density is greatly lowered, therefore, adopt the solaode that the polycrystal silicon ingot that the embodiment of the present invention provides is produced, monocrystaline silicon solar cell attenuation quotient more of the prior art is lower, and polysilicon solar cell photoelectric transformation efficiency more of the prior art is higher.
And, owing to the present embodiment adopting the mode of repeatedly melt back crystallization form polycrystal silicon ingot, be equivalent to slow down to a certain extent the fractional condensation speed of the setting rate of crystal and impurity on the whole, make impurity (such as carborundum, silicon nitride etc.) there is time enough and fractional condensation can be carried out fully, even if the impurity precipitated out in advance, in follow-up methback process, can also again be dissolved in silicon liquid, thus avoiding impurity to be deposited in the crystalline region solidified, and then decrease the impurity content in cast main body, improve minority carrier life time, thus improve the electricity conversion of solaode.
Embodiment two
The flow chart of the casting method of the polycrystal silicon ingot disclosed in the present embodiment as it is shown on figure 3, with a upper embodiment the difference is that, the process that will load silicon raw material in the present embodiment embodies, and the method comprises the following steps:
Step S201: the container bottom in polycrystal silicon ingot growth furnace, the seed crystal splicing tiling adopting crystalline orientation identical forms described inculating crystal layer, and described inculating crystal layer is substantially parallel with described container bottom;
The present embodiment is preferably the monocrystal silicon tiling adopting (100) orientation and forms described inculating crystal layer, preferably, the area of described inculating crystal layer occupies the percentage ratio of described container bottom area, namely the area of described inculating crystal layer occupies the percentage ratio of described container bottom area is 50%-99%, preferred, the area of described inculating crystal layer occupies the 70%-99% of described container bottom area, preferred, the area of described inculating crystal layer occupies the 90%-99% of described container bottom area, preferred, the area of described inculating crystal layer occupies the 95%-99% of described container bottom area.
Step S202: short grained silicon raw material is loaded into the top of described inculating crystal layer, to fill the gap between described seed crystal and the gap between described inculating crystal layer and described container side wall;
Owing to adopting the seed crystal paving of fritter to form inculating crystal layer in the present embodiment, consider paving process can there will be gap between the position and inculating crystal layer and container side wall of splicing seams, in casting process, these gaps are easily caused in cast main body and the defects such as hole occur, thus affecting product quality, adopt short grained silicon raw material blind, the cavity blemish in cast main body can be avoided on the one hand, the foreign gas in gap can also be got rid of, to reduce swirl defect and various oxygen triggering holes etc., and also can utilize little granular silicon feedstock there is bigger specific surface area, it is relatively easy to endothermic melting advantage, blind, the impurity such as the oxygen that can better stop container bottom.
Step S203: the silicon raw material of large volume is loaded into the top of described little granular silicon feedstock, until container (crucible) is filled, namely completes the loading process of silicon raw material.
The present embodiment completes the laden schematic diagram of silicon raw material as shown in Figure 4 and Figure 5, Fig. 4 is top view, the inculating crystal layer formed by monocrystal silicon 21 paving of (100) orientation in figure is surrounded by silicon raw material 22, Fig. 5 is profile, inculating crystal layer 23 is arranged above short grained silicon raw material 24, top is the silicon raw material 26 of large volume again, and not directly and the sidewall contact of crucible 25, the gap between the sidewall of inculating crystal layer 23 and crucible 25 has little granular silicon feedstock 24 to fill to inculating crystal layer 23.
Performing step S204-step S206 afterwards, described silicon raw material and part inculating crystal layer melt-crystallization-melt back crystallization process, this process is similar with the step S103-step S105 in a upper embodiment, repeats no more here.
The profile of the polycrystal silicon ingot that the method for employing the present embodiment is produced is as shown in Figure 6, the mid portion of this polycrystal silicon ingot is monocrystalline silicon region 31, monocrystalline silicon region 31 has consistent crystalline orientation with seed crystal below, around monocrystalline silicon region 31, owing in sidewall of crucible 32, impurity is more, the very easily reason of nucleation, therefore around monocrystalline silicon region 31, form the polysilicon region 33 that crystalline orientation is random, unfused inculating crystal layer 23 is also had in crucible bottom, owing to having gap between the seed crystal of paving, what fill between gap is short grained silicon raw material, thus there is crystal boundary 34 between the monocrystalline silicon region 31 of the polycrystal silicon ingot produced, but owing to the chip area of monocrystalline silicon region 31 is big, therefore, polycrystal silicon ingot more of the prior art, the density of the crystal boundary 34 of the polycrystal silicon ingot made in the present embodiment greatly reduces.
Embodiment three
Present embodiment discloses the polycrystal silicon ingot adopting the method for various embodiments above to produce and the solar wafer adopting the polycrystal silicon ingot produced to make and solaode.
Wherein, described polycrystal silicon ingot comprises continuous large-sized monocrystalline silicon region that crystalline orientation is consistent, after the impurity enriched layer at described polycrystal silicon ingot two ends is excised, other body region is carried out cutting and obtains solar wafer, utilizing described wafer fabrication solaode, described solaode includes:
Wafer, described wafer has continuous large-sized monocrystalline silicon region that crystalline orientation is consistent;
P-N junction in described wafer;
Conductive contact on described wafer.
Comprise in addition coating antireflective coating on the wafer, to reduce the wafer reflection to light, strengthen the absorption to light.
In polycrystal silicon ingot in the present embodiment, the content of oxygen, carbon and other impurity is all relatively low, and the defects such as grain boundary density are substantially reduced, owing to the Hard Inclusion in cast main body having been carried out good control in production process, therefore the defect concentration in cast main body is greatly reduced.
Wafer owing to obtaining has the monocrystalline silicon region that the crystalline orientation of continuous large-area is consistent, therefore chemical method preferential etch pyramid matte can be adopted, wafer surface is carried out good texture, increase the absorption to light, and, grain boundary density relatively low in wafer, it is possible to effectively avoid because of the low defect of the photoelectric transformation efficiency of the too high solar battery sheet caused of the grain boundary density in material.
In sum, relative to monocrystaline silicon solar cell of the prior art, solaode in the present embodiment has less attenuation quotient, and relative to polysilicon solar cell of the prior art, the solaode in the present embodiment has higher photoelectric transformation efficiency.
In this specification, various piece adopts the mode gone forward one by one to describe, and what each some importance illustrated is the difference with other parts, between various piece identical similar portion mutually referring to.
Described above to the disclosed embodiments, makes professional and technical personnel in the field be capable of or uses the present invention. The multiple amendment of these embodiments be will be apparent from for those skilled in the art, and generic principles defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments. Therefore, the present invention is not intended to be limited to embodiment illustrated herein, and is to fit to the widest scope consistent with principles disclosed herein and features of novelty.
Claims (10)
1. the manufacture method of a polycrystal silicon ingot, it is characterised in that including:
Container bottom in polycrystal silicon ingot growth furnace lays seed crystal, forms inculating crystal layer, described inculating crystal layer and described container bottom keeping parallelism;
The silicon raw material of solid-state is loaded into the top of described inculating crystal layer;
Described container being heated, melts described silicon raw material and the described inculating crystal layer of part, to form liquid level, at least keeping the part inculating crystal layer contacted with described container bottom is solid-state;
Control the thermal field in described polycrystal silicon ingot growth furnace, described liquid level is carried out crystallization and forms crystallizing layer, so that solid liquid interface moves to the direction away from described container bottom;
After described solid liquid interface moves respective distance to the direction away from described container bottom, enter melt back crystallization process, after at least performing once described melt back crystallization process, obtain polycrystal silicon ingot;
Wherein, described melt back crystallization process includes, control the thermal field in described polycrystal silicon ingot growth furnace, described crystallizing layer is carried out melt back, described solid liquid interface is made to move to the direction near described container bottom, afterwards, control the thermal field in described polycrystal silicon ingot growth furnace, liquid level is carried out crystallization, so that described solid liquid interface moves to the direction away from described container bottom, make every subcrystalline height height more than melt back, the distance that the distance that described solid liquid interface moves to the direction near described container bottom moves to the direction away from described container bottom less than described solid liquid interface.
2. the manufacture method of polycrystal silicon ingot according to claim 1, it is characterised in that described polycrystal silicon ingot contains the large-sized monocrystalline silicon region of continuous print, the crystalline orientation of described monocrystalline silicon region is identical with the crystalline orientation of the described seed crystal being disposed below.
3. the manufacture method of polycrystal silicon ingot according to claim 1, it is characterised in that described seed crystal is crystalline orientation is the monocrystal silicon of (100), (110) or (111).
4. the manufacture method of polycrystal silicon ingot according to claim 1, it is characterised in that the silicon raw material of solid-state is loaded into the process of the top of described inculating crystal layer particularly as follows:
Short grained silicon raw material is loaded into the top of described inculating crystal layer, to fill the gap between described seed crystal and the gap between described inculating crystal layer and described container side wall;
The silicon raw material of large volume is loaded into the top of described little granular silicon feedstock.
5. the manufacture method of polycrystal silicon ingot according to claim 1, it is characterised in that the thickness of described inculating crystal layer is 10mm-100mm.
6. the manufacture method of polycrystal silicon ingot according to claim 5, it is characterised in that when first time starts crystallization, the thickness of solid seed crystal layer is 1mm-50mm.
7. the manufacture method of polycrystal silicon ingot according to claim 1, it is characterised in that the area of described inculating crystal layer occupies the 50%-99% of described container bottom area.
8. the manufacture method of polycrystal silicon ingot according to claim 1, it is characterised in that described container is silica crucible, silicon carbide crucible or silicon nitride crucible.
9. the polycrystal silicon ingot that the method adopted described in any one of claim 1-8 is produced, it is characterised in that described polycrystal silicon ingot comprises continuous large-sized monocrystalline silicon region that crystalline orientation is consistent.
10. a solaode, adopts the polycrystal silicon ingot described in claim 9, it is characterised in that including:
Wafer, described wafer has continuous large-sized monocrystalline silicon region that crystalline orientation is consistent;
P-N junction in described wafer;
Conductive contact on described wafer.
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| CN103510157B (en) * | 2013-10-09 | 2016-03-02 | 青岛隆盛晶硅科技有限公司 | A kind of long brilliant technique of induction of efficient ingot casting |
| TWI548784B (en) * | 2014-01-16 | 2016-09-11 | 中美矽晶製品股份有限公司 | Crucible assembly and method of manufacturing crystalline silicon ingot by use of such crucible assembly |
| CN104894642A (en) * | 2015-06-29 | 2015-09-09 | 韩华新能源（启东）有限公司 | Method for improving quality of casted polycrystalline silicon ingots |
| CN106245113B (en) * | 2016-09-18 | 2018-10-19 | 江西赛维Ldk太阳能高科技有限公司 | A kind of polycrystal silicon ingot and preparation method thereof and polysilicon chip |
| CN107740185A (en) * | 2017-11-06 | 2018-02-27 | 晶科能源有限公司 | The shop fixtures method of one species single crystal seed |
| CN115012035B (en) * | 2022-06-02 | 2024-06-14 | 金阳(泉州)新能源科技有限公司 | Preparation method of cast crystalline silicon with dislocation defect and polycrystalline duty ratio reduced |
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