CN104313688A - Method for adjusting crystalline silica growth solid-liquid interface - Google Patents
Method for adjusting crystalline silica growth solid-liquid interface Download PDFInfo
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- CN104313688A CN104313688A CN201410469582.8A CN201410469582A CN104313688A CN 104313688 A CN104313688 A CN 104313688A CN 201410469582 A CN201410469582 A CN 201410469582A CN 104313688 A CN104313688 A CN 104313688A
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- crucible
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/04—Production of homogeneous polycrystalline material with defined structure from liquids
- C30B28/06—Production of homogeneous polycrystalline material with defined structure from liquids by normal freezing or freezing under temperature gradient
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- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
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- Organic Chemistry (AREA)
- Silicon Compounds (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a method for adjusting a crystalline silica growth solid-liquid interface. The method can be realized by two approaches. The two approaches comprise 1, designing four side walls having different thickness values of a crucible, and 2, changing sides of thermal insulation strips at sides of a thermal insulation cage in an ingot furnace thermal field and accordingly changing an ingot casting technology. The method solves the problem that crystal growth solid-liquid interface change causes silicon ingot quality decreasing so that photoelectric conversion efficiency of a crystalline silica solar cell piece is improved.
Description
Technical field
The present invention relates to a kind of method adjusting the long brilliant solid-liquid interface of crystalline silicon, belong to solar-photovoltaic technology field.
Background technology
Solar energy power generating is one of form of utilizing of sustainable energy with fastest developing speed at present, along with to the demand of solar cell with annual about tens percent speed increase, the demand of polycrystalline silicon used for solar battery ingot is also increase considerably every year.Modern photovoltaic industry more than 85% is based on crystal silicon chip solar cell, and wherein employing directionally solidified crystal silicon materials over half manufacture.In directional freeze process, the quality of solid-liquid interface to crystal mass of crystal plays conclusive effect.In directional freeze process, the quality of solid-liquid interface to crystal mass of crystal plays conclusive effect, mainly due to ceramic crucible in long brilliant process and graphite protective plate all very thin, corresponding heat-sinking capability is higher than heat exchange platform, to such an extent as to need dispersed heat during crystal growth mainly through the sidewall of crucible of surrounding and plumbago crucible to external diffusion, this is by the speed that causes reducing near the silicon melt temperature of the surrounding crucible silicon melt much larger than crucible bottom, and the crystalline silicon contacted with sidewall of crucible is in the long brilliant diffusion of stage in the middle part of silicon ingot, growth.Therefore the ingot furnace used now is in long brilliant process, and most of solid-liquid interface is all in W type interface, and being applicable to long brilliant convex interface with present generally acknowledged comparing has certain difference, is unfavorable for the eliminating of the impurity in silicon ingot like this.
Solid-liquid interface is unstable, directly results in the fluctuation of crystalline silicon ingot quality.Most of enterprise of current production crystalline silicon not only solid-liquid interface entirety is W type interface, but also the heterogeneity phantom that all can run into ingot furnace uneven phenomenon, this thermal field is uneven directly results in solid-liquid interface not to lining.Therefore, seek a kind ofly the method for adjusting and optimizing solid-liquid interface targetedly to seem particularly important.
Summary of the invention
The object of this invention is to provide a kind of method adjusting the long brilliant solid-liquid interface of crystalline silicon, realize by two kinds of approach.1: be different thickness by four Design of Side Walls of crucible.2: change heat-insulation cage sidepiece heat preservation strip in ingot furnace thermal field size and in conjunction with the change of casting ingot process.By optimizing the long brilliant solid-liquid interface of crystal, improving polycrystalline silicon ingot casting quality, improving photoelectric transformation efficiency.
A kind ofly adjust improving one's methods of the long brilliant solid-liquid interface of crystalline silicon, be specially the size changing crucible: institute adopts crucible material to be quartzy or silicon nitride, and crucible is square, and comprises four abutment walls and a bottom surface, and the thickness of four abutment walls of crucible arranges inconsistent.
A kind ofly adjust improving one's methods of the long brilliant solid-liquid interface of crystalline silicon, be specially the size that changes heat-insulation cage sidepiece heat preservation strip in ingot furnace thermal field and in conjunction with the change of casting ingot process: ingot furnace comprises upper furnace body, thermal baffle, side heat-insulation cage, well heater, graphite protective plate, heat exchange mass, lower furnace body, heat preservation strip, end thermal baffle, ceramic crucible, crucible cover plate, lifting connecting rod, electrode; Upper furnace body and lower furnace body are connected to form whole body of heater, ceramic crucible is provided with in body of heater, crucible cover plate is placed on ceramic crucible, be provided with graphite protective plate outside ceramic crucible, be provided with heat exchange mass below ceramic crucible, well heater is connected with upper furnace body by electrode, side heat-insulation cage is connected with upper furnace body by promoting connecting rod, heat-insulation cage top, side is provided with thermal baffle, and side heat-insulation cage bottom sides is provided with heat preservation strip, is provided with end thermal baffle bottom the heat-insulation cage of side.
Preferably, the heat preservation strip difference in height scope being arranged on heat-insulation cage bottom sides is 0-50mm, and width difference scope is 0-15mm.
Preferably, the altitude range of heat preservation strip is 10-140mm, and width range is 10-70mm.
Preferably, the altitude range of heat preservation strip is 100-140mm, ingot melting and long brilliant technological temperature rising 1-12 DEG C during ingot casting.
The invention has the beneficial effects as follows: present method solves long brilliant solid-liquid interface targetedly and changes the problem causing crystal mass to decline, not only reduce the inner dislocation desity of silicon ingot, foreign matter content and ingot casting yield rate is increased further, finally improving the photoelectric transformation efficiency of crystal silicon solar cell sheet.
Accompanying drawing explanation
Fig. 1 is crucible schematic diagram.
Reference numeral: side 110, side 120, side 130, side 140, bottom surface 150.
Fig. 2 is silicon ingot longitudinal section solid-liquid interface PL scintigram before the adjustment of embodiment 1 crucible wall.
Fig. 3 is silicon ingot longitudinal section solid-liquid interface PL scintigram after the adjustment of embodiment 1 crucible wall.
Fig. 4 is ingot furnace schematic diagram.
Reference numeral: upper furnace body 1, thermal baffle 2, side heat-insulation cage 3, well heater 4, graphite protective plate 5, heat exchange mass 6, lower furnace body 7, heat preservation strip 8, end thermal baffle 9, ceramic crucible 10, crucible cover plate 11, lifting connecting rod 12, electrode 13.
Fig. 5 is silicon ingot longitudinal section solid-liquid interface PL scintigram before the adjustment of sidepiece heat preservation strip.
Fig. 6 is silicon ingot longitudinal section solid-liquid interface PL scintigram after the adjustment of sidepiece heat preservation strip.
Embodiment
In order to be that those skilled in the art person better understands patent formula of the present invention, and above-mentioned purpose of the present invention, feature and advantage be become apparent, be described in further details below in conjunction with embodiment.
Embodiment 1
Adjust a method for the long brilliant solid-liquid interface of crystalline silicon, with common lift heat insulation cage GT450 directional solidification polysilicon stove growing polycrystalline silicon ingot.Adopt crucible material be high purity quartz pottery, be of a size of 880*880*420mm.Design crucible, side 110, side 120, side 130, side 140, bottom surface 150 thickness is designed to 22mm, 22mm successively, 26mm, 22mm, 23mm, the wall thickness of corresponding side surface 130 is increased to 26mm by original 22mm, in crucible, fill silicon material 485kg, successively through fusion stage → length brilliant stage → annealing stage → cooling stages.By after silicon ingot vertical profile after ingot casting completes, the LIS-R1 photoluminescence tester produced with BTI company detects the longitudinal section of 5 little side's ingots corresponding to silicon ingot medullary ray, after splicing, observe the shape of solid-liquid interface, grain growing direction and the black surround situation near crucible edge regions.
As accompanying drawing 1, do not adjust the crucible before crucible wall thickness, this thermal field right side area, the direction of growth (as shown by arrows in FIG.) of column crystal is larger to silicon ingot inside extension slope, and the slope that the direction of growth of left side crystal grain extends to silicon ingot inside is less, the black surround situation on right side and dislocation are from also obvious also more than the left side, obviously there is thermal field non-uniform phenomenon, by increasing the crucible wall thickness of right side area, make in the long brilliant stage, relative improves the temperature of right side near crucible melt, and solid-liquid interface concavity is herein reduced.Silicon ingot longitudinal diagram after adjustment as shown in Figure 2, dislocation reduces from quantity, before dislocation desity is starkly lower than adjustment, because the concavity near crucible region solid-liquid interface reduces, the slope that the direction of growth of right side crystal grain internally tilts obviously reduces, left and right sides almost symmetry, black surround region reduces, through infra-red inspection tester (Semilab IRB-50), minority carrier lifetime tester (Semilab WT-2000PVN) is tested silicon ingot, data are as shown in table 1, silicon ingot foreign matter content ratio after adjustment reduces by 1.98%, ingot casting yield improves 3.44%, for confirming the reduction of foreign matter content further, adopt inductively coupled plasma atomic mass spectrometry, measure the average body metal content of silicon ingot, as shown in table 2, the body metal content decline 59.64ppb of silicon ingot, Ingot quality significantly improves.
Before and after table 1 adjusts, ingot casting detects Data Comparison:
Silicon ingot body metals content impurity contrast before and after table 2 adjusts:
Embodiment 2
Improving one's methods of brilliant solid-liquid interface grown by a kind of crystalline silicon that adjusts, and is specially the shape of the heat preservation strip changing heat-insulation cage sidepiece in ingot furnace, size and casting ingot process: ingot furnace comprises upper furnace body 1, thermal baffle 2, side heat-insulation cage 3, well heater 4, graphite protective plate 5, heat exchange mass 6, lower furnace body 7, heat preservation strip 8, end thermal baffle 9, attemperator 10, ceramic crucible 11, promotes connecting rod 12, electrode 13; Upper furnace body 1 and lower furnace body 7 are connected to form whole body of heater, ceramic crucible 10 is provided with in body of heater, crucible cover plate 11 is placed on ceramic crucible 10, be provided with graphite protective plate 5 outside ceramic crucible 10, be provided with heat exchange mass 6 below ceramic crucible 10, well heater 4 is connected with upper furnace body 1 by electrode 13, side heat-insulation cage 3 is connected with upper furnace body 1 by promoting connecting rod 12, side heat-insulation cage 3 top is provided with thermal baffle 2, and side heat-insulation cage 3 bottom sides is provided with heat preservation strip 8, is provided with end thermal baffle 9 bottom side heat-insulation cage 3.
In the present embodiment, in order to improve the ununiformity of left side thermal field and overall solid-liquid interface shape, the sidepiece heat preservation strip 8 of surrounding is designed to 1132 × 65 × 120mm, 1132 × 60 × 100mm, 1132 × 60 × 100mm, 1132 × 60 × 100mm, make it form ring-type round ceramic crucible.Crucible material that the present embodiment adopts is high purity quartz pottery, is of a size of 880 × 880 × 420mm, fills silicon material 485kg in crucible.
As accompanying drawing 5, before not adjusting, overall solid-liquid interface is W shape, and this thermal field left field, the direction of growth (as shown by arrows in FIG.) of column crystal is larger to silicon ingot inside extension slope, in former DSS GT450 directional solidification polysilicon stove, sidepiece heat preservation strip is of a size of 1132 × 60 × 45mm, and after increasing heat preservation strip, Base Heat board dispersed heat increases, for guaranteeing that long crystalline substance normally carries out, increase long brilliant temperature.Silicon material successively through fusion stage → length brilliant stage → annealing stage → cooling stages.By after silicon ingot vertical profile after ingot casting completes, the LIS-R1 photoluminescence tester produced with BTI company detects the longitudinal section of 5 little side's ingots corresponding to silicon ingot medullary ray, after splicing, observe the shape of solid-liquid interface, grain growing direction and the black surround situation near crucible edge regions.
As accompanying drawing 5, when not adopting new design heat preservation strip, solid-liquid interface is W type interface, is caused the change of solid-liquid interface after installing this heat preservation strip by the increase of Base Heat board dispersed heat.After adjustment, silicon ingot longitudinal diagram as shown in Figure 6, solid-liquid interface in long brilliant process changes convex interface into by W type interface, the silicon ingot grain growing direction in B district becomes outward-dipping from original to silicon ingot inner inclination, contrast two pictures, the dislocation of accompanying drawing 6 obviously reduces from quantity, and dislocation desity reduces.Convex interface is also conducive to impurities removal, near the black surround region also corresponding minimizing of crucible.Through infra-red inspection tester (Semilab IRB-50), minority carrier lifetime tester (Semilab WT-2000PVN) is tested silicon ingot, data are as shown in table 5, silicon ingot foreign matter content ratio after adjustment reduces by 1.82%, ingot casting yield improves 3.58%, for confirming the reduction of foreign matter content further, inductively coupled plasma atomic mass spectrometry is adopted to measure the average body metals content impurity of silicon ingot, as shown in table 6, the body metal content of silicon ingot does not adjust front decline 68.42ppb, obviously reduces.
The 2 long brilliant techniques in routine Central Plains implemented by table 3
The brilliant technique of length in table 4 embodiment 2 after adjustment
Before and after table 5 adjusts, ingot casting detects Data Comparison:
Silicon ingot body metals content impurity contrast before and after table 6 adjusts:
Claims (6)
1. adjust a method for the long brilliant solid-liquid interface of crystalline silicon, it is characterized in that, by changing the size of crucible or changing the shape of heat preservation strip of side heat-insulation cage bottom sides in ingot furnace, size and casting ingot process and realize.
2. a kind of method adjusting the long brilliant solid-liquid interface of crystalline silicon as claimed in claim 1, it is characterized by: be specially and change the size of crucible: institute adopts crucible material to be quartzy or silicon nitride, crucible is square, and comprise four abutment walls and a bottom surface, the thickness of four abutment walls of crucible arranges inconsistent.
3. a kind of method adjusting the long brilliant solid-liquid interface of crystalline silicon as claimed in claim 1, is characterized by: be specially the shape of the heat preservation strip changing side heat-insulation cage bottom sides in ingot furnace, size and casting ingot process: ingot furnace comprises upper furnace body (1), thermal baffle (2), side heat-insulation cage (3), well heater (4), graphite protective plate (5), heat exchange mass (6), lower furnace body (7), heat preservation strip (8), end thermal baffle (9), attemperator (10), ceramic crucible (11), promotes connecting rod (12), electrode (13), upper furnace body (1) and lower furnace body (7) are connected to form whole body of heater, ceramic crucible (10) is provided with in body of heater, crucible cover plate (11) is placed on ceramic crucible (10), ceramic crucible (10) outside is provided with graphite protective plate (5), ceramic crucible (10) below is provided with heat exchange mass (6), well heater (4) is connected with upper furnace body (1) by electrode (13), side heat-insulation cage (3) is connected with upper furnace body (1) by promoting connecting rod (12), side heat-insulation cage (3) top is provided with thermal baffle (2), side heat-insulation cage (3) bottom sides is provided with heat preservation strip (8), side heat-insulation cage (3) bottom is provided with end thermal baffle (9).
4. a kind of method adjusting the long brilliant solid-liquid interface of crystalline silicon as claimed in claim 3, is characterized by: the heat preservation strip difference in height scope being arranged on heat-insulation cage bottom sides is 0-50mm, and width difference scope is 0-15mm.
5. a kind of method adjusting the long brilliant solid-liquid interface of crystalline silicon as claimed in claim 3, is characterized by: the altitude range of heat preservation strip is 10-140mm, and width range is 10-70mm.
6. a kind of method adjusting the long brilliant solid-liquid interface of crystalline silicon as claimed in claim 3, is characterized by: the altitude range of heat preservation strip is 100-140mm, and during ingot casting, the long brilliant technological temperature of ingot casting raises 1-12 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410469582.8A CN104313688A (en) | 2014-09-16 | 2014-09-16 | Method for adjusting crystalline silica growth solid-liquid interface |
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| CN201410469582.8A CN104313688A (en) | 2014-09-16 | 2014-09-16 | Method for adjusting crystalline silica growth solid-liquid interface |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109112617A (en) * | 2017-06-23 | 2019-01-01 | 镇江仁德新能源科技有限公司 | A kind of directional solidification furnace and directional freeze method of solar energy polycrystalline silicon |
| CN111394790A (en) * | 2020-04-26 | 2020-07-10 | 新余学院 | Low-impurity polycrystalline silicon ingot furnace |
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| CN101775641A (en) * | 2010-02-09 | 2010-07-14 | 宁波晶元太阳能有限公司 | Follow-up heat insulation ring thermal field structure for vertical oriented growth of polysilicon |
| CN102108544A (en) * | 2010-10-08 | 2011-06-29 | 常州天合光能有限公司 | Thermal field structure used in polycrystalline silicon ingot furnace for controlling crystal growth interface |
| CN102644104A (en) * | 2011-06-15 | 2012-08-22 | 安阳市凤凰光伏科技有限公司 | Gradient improving device of thermal field for producing pseudo single crystal silicon ingot by casting method |
| CN202755096U (en) * | 2012-03-19 | 2013-02-27 | 江苏协鑫硅材料科技发展有限公司 | Heat insulation device for ingot furnace |
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2014
- 2014-09-16 CN CN201410469582.8A patent/CN104313688A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101775641A (en) * | 2010-02-09 | 2010-07-14 | 宁波晶元太阳能有限公司 | Follow-up heat insulation ring thermal field structure for vertical oriented growth of polysilicon |
| CN102108544A (en) * | 2010-10-08 | 2011-06-29 | 常州天合光能有限公司 | Thermal field structure used in polycrystalline silicon ingot furnace for controlling crystal growth interface |
| CN102644104A (en) * | 2011-06-15 | 2012-08-22 | 安阳市凤凰光伏科技有限公司 | Gradient improving device of thermal field for producing pseudo single crystal silicon ingot by casting method |
| CN202755096U (en) * | 2012-03-19 | 2013-02-27 | 江苏协鑫硅材料科技发展有限公司 | Heat insulation device for ingot furnace |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109112617A (en) * | 2017-06-23 | 2019-01-01 | 镇江仁德新能源科技有限公司 | A kind of directional solidification furnace and directional freeze method of solar energy polycrystalline silicon |
| CN111394790A (en) * | 2020-04-26 | 2020-07-10 | 新余学院 | Low-impurity polycrystalline silicon ingot furnace |
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