CN109402733A - A kind of preparation method of the efficient silicon ingot of fine melt of low metal pollution - Google Patents
A kind of preparation method of the efficient silicon ingot of fine melt of low metal pollution Download PDFInfo
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- CN109402733A CN109402733A CN201811124472.2A CN201811124472A CN109402733A CN 109402733 A CN109402733 A CN 109402733A CN 201811124472 A CN201811124472 A CN 201811124472A CN 109402733 A CN109402733 A CN 109402733A
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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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- 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
Abstract
The invention discloses a kind of preparation methods of the efficient silicon ingot of fine melt of low metal pollution, including following below scheme: the high active layer production in high-purity layer of production-bottom of crucible bottom-silicon nitride release layer spraying-charging-ingot casting, the present invention preparation method is by increasing high-purity layer in crucible bottom, promote high active layer quartz sand purity and silicon nitride release layer purity, having achieved the purpose that, which reduces metal impurities, pollutes silicon ingot, promote silicon ingot yield, by reducing pollution of the metallic iron to silicon ingot in crucible, the generation probability for reducing B-Fe complex, reaching reduces silicon wafer light decay rate.
Description
Technical field
The present invention relates to a kind of preparation methods of the efficient silicon ingot of fine melt of low metal pollution, belong to field of polycrystalline silicon ingot.
Background technique
Currently, the preparation method of polycrystal silicon ingot is mainly prepared using the directional solidification system that GT Solar is provided,
This method generally include heating, fusing, it is long brilliant, anneal and cool down, during solidification is long brilliant, by head temperature
It is controlled with side insulation cover aperture, so that melting silicon liquid obtains enough degree of supercooling solidification and crystallizations in crucible bottom, due to
Conventional polycrystalline ingot casting, bottom forming core are random spontaneous nucleation, are unable to get effective control, generate for conventional foundry ingot mode more
Crystal silicon ingot has that forming core is unable to control, silicon ingot inside dislocation density is high, crystal boundary is more and random distribution, polysilicon technology personnel
Be proposed three kinds of different types of polycrystalline cast ingot modes based on the considerations of control forming core: one of which is to be grown using monocrystal seeding
Principle, in crucible bottom be laid with monocrystalline plate or block as growth seed crystal, control forming core forms class monocrystalline silicon piece, represents producer
Such as assist prosperous, phoenix photovoltaic and sunlight brightness；The second way is to be laid with broken silicon material as growth seed crystal in crucible bottom, controls shape
Karyomorphism has the high-efficiency polycrystalline silicon wafer of fine grain structure, the typical products such as A4+ silicon wafer of Taiwan Sino-U.S. silicon crystal, match at surface
Prosperous S2, S3 silicon wafer etc. of the M3 silicon wafer of dimension, association；The third mode is similar to the second way, but bottom is made with broken silicon material
It for forming core source, but utilizes bottom to be laid with quartz sand and cooperates suitable spraying casting ingot process, ultimately form carry out fine particle, reach
To reduction dislocation, the target of raising efficiency, the H3+ of Typical Representative such as ring too, the R3 silicon wafer of Rong De.
Above-mentioned three kinds of modes effectively improve the photoelectric conversion efficiency of polycrystal silicon ingot by different control nucleation modes,
The photoelectric conversion efficiency of class monocrystalline silicon piece and crystal grain high-efficiency polycrystalline silicon wafer fine crushing is 16.8% ~ 17.0% or so big by ordinary silicon chip
Width is promoted between 18.6% ~ 18.9%, but there is also following problems:
1, class monocrystalline silicon piece due to single crystal seed it is expensive, at high cost, dislocation is high, cannot achieve volume production；
2, efficiently since bottom silicon material not exclusively melts, ingot casting yield is low, at high cost for fritting；
3, the third scheme is currently the efficient silicon wafer fabrication scheme of economical and efficient the most, but silicon ingot is directly contacted with crucible, is led
Cause metal impurities diffusion breadth wide (4us or less width is in 45mm or so), ingot casting yield is relatively relatively low, and B-Fe composite principle,
Cause light decay high, for further pushing photovoltaic cheap internet access to cause obstruction；Therefore, researching and developing a kind of can overcome disadvantages described above
The preparation method of efficient silicon ingot becomes those skilled in the art's technical problem urgently to be resolved.
Summary of the invention
The technical problem to be solved by the present invention is to, the shortcomings that overcoming the prior art, a kind of the complete of low metal pollution is provided
The preparation method of efficient silicon ingot is melted, which promotes high active layer quartz sand purity by increasing high-purity layer in crucible bottom
With silicon nitride release layer purity, having achieved the purpose that, which reduces metal impurities, pollutes silicon ingot, silicon ingot yield is promoted, by reducing earthenware
Pollution of the metallic iron to silicon ingot in crucible reduces the generation probability of B-Fe complex, and reaching reduces silicon wafer light decay rate.
In order to solve the above technical problems, the present invention provides a kind of preparation side of the efficient silicon ingot of fine melt of low metal pollution
Method, including following below scheme: the high active layer production in high-purity layer of production-bottom of crucible bottom-silicon nitride release layer spraying-charging-ingot casting,
Wherein:
(1) high-purity layer of crucible bottom production
The tekite sand collocation of high purity crystalline sand of the tenor no more than 2ppm and tenor no more than 5ppm is mixed
It closes, according to quality than high purity crystalline sand: tekite sand=3:7-5:5, the high purity quartz slurry for being then milled to partial size 5-10um are molten
Liquid, resulting high purity quartz slurry solution solid phase ratio is in 30%-40%；
The high purity quartz slurry solution of acquisition is brushed using the method brushed in crucible surface, every crucible high purity quartz slurry
Solution usage in 800-1000g, after be put into tunnel kiln drying, drying temperature is 50-60 DEG C, drying time 1-2h, then
It takes out and places to room temperature, form high-purity layer in crucible bottom；
(2) the high active layer production in bottom
A. high purity quartz obtained in step (1) is starched into solution, is diluted using silica solution as the bonding of the high active layer in bottom
Agent, wherein meter high purity quartz in mass ratio starches solution: silica solution=3:7,
B. the binder of the high active layer in bottom obtained is brushed in the way of brushing or spraying high-purity made from step (1)
On layer, it is rear using spread painting in the way of mesh number is spread to crucible bottom for the efficient sand of 50-80 mesh, form high active layer；
(3) silicon nitride release layer sprays
Silicon nitride release layer is made of silicon nitride, pure water and silica solution, in mass ratio meter silicon nitride: pure water: silica solution=1:
2.5-3.5:0.5；
Silicon nitride in silicon nitride release layer is by Ah method's Phase Proportion >=95%, tenor≤1ppm specification silicon nitride and A Fa
Phase Proportion is mixed in 50%-60%, tenor≤3ppm specification silicon nitride according to mass ratio 1:1-2:1；
The mixture of silicon nitride release layer is sprayed into inner surface of crucible in the way of spraying, 80-95 DEG C of spraying temperature, is sprayed
Enclose number 20-26 circle；
(4) it charges
Loading stage, according to conventional charging method, first seed crystal small powder-reclaimed materials-routine block step, by weight in 0.8-
The silicon material of 0.9T is charged in crucible；
(5) ingot casting
G6 silicon material is packed into G6 polycrystalline furnace according to old process, by normal occlusion stove evacuation after dress heat preservation strip, is heated to 1560 DEG C,
So that after silicon material is melted completely, by controlling the top central region temperature (TC1) and heat-insulation cage aperture of ingot casting, into long brilliant rank
Section, until long brilliant completion.
The technical solution that the present invention further limits is:
Further, in the preparation method of the efficient silicon ingot of fine melt of aforementioned low metal pollution, Fe content≤1ppm in silica solution, Gu
Phase content 30%.
In the preparation method of the efficient silicon ingot of fine melt of aforementioned low metal pollution, the crucible of use is having a size of 1060*1060*
When the G6 crucible of 540mm, the control of silicon nitride dosage exists in silicon nitride release layer when silicon nitride release layer sprays in step (3)
800-900g。
The beneficial effects of the present invention are:
Big for bottom metal impurities diffusion breadth in fine melt efficient scheme in the prior art, B-Fe is compound to cause silicon wafer light decay high
The problem of, the present invention is mainly improved from the following aspects:
1) add in conventional high-performance crucible bottom and brushed one layer of high-purity layer of high-purity impurity barrier layer；
2) the higher quartz sand of purity is used instead for the high active layer in bottom, reduce high active layer and the impurity of silicon ingot is polluted；
3) bottom nitride silicon release layer introduces nitrogen for ultra-high purity SiClx as release layer, reduces dirt of the release layer impurity to silicon ingot
Dye；
The present invention promotes high active layer quartz sand purity and silicon nitride release layer purity, reaches by increasing high-purity layer in crucible bottom
Having arrived reduces the purpose that metal impurities pollute silicon ingot, and brilliant brick bottom red sector reduces 10mm or more, and it is left to promote silicon ingot yield 2.5%
It is right；By reducing pollution of the metallic iron to silicon ingot in crucible, reduce the generation probability of B-Fe complex, reaching reduces silicon wafer light
Decline 1% or more.
Detailed description of the invention
Fig. 1 is few sub- detection figure of silicon ingot in the prior art；
Fig. 2 is few sub- detection figure of silicon ingot in the embodiment of the present invention.
Specific embodiment
Embodiment 1
A kind of preparation method of the efficient silicon ingot of fine melt of low metal pollution provided in this embodiment, including following below scheme: crucible bottom
The production of high-purity layer of portion, the high active layer production in bottom, the spraying of silicon nitride release layer, charging, ingot casting, in which:
(1) high-purity layer of crucible bottom production
The tekite sand collocation of high purity crystalline sand of the tenor no more than 2ppm and tenor no more than 5ppm is mixed
It closes, according to quality than high purity crystalline sand: tekite sand=3:7 is then milled to the high purity quartz slurry solution of partial size 5um, gained
High purity quartz slurry solution solid phase ratio 30%；
The high purity quartz slurry solution of acquisition is brushed using the method brushed in crucible surface, every crucible high purity quartz slurry
Solution usage in 800g, after be put into tunnel kiln drying, drying temperature is 50 DEG C, drying time 1h, then takes out placement extremely
Room temperature forms high-purity layer in crucible bottom；
(2) the high active layer production in bottom
A. high purity quartz obtained in step (1) is starched into solution, is diluted using silica solution as the bonding of the high active layer in bottom
Agent, wherein meter high purity quartz in mass ratio starches solution: silica solution=3:7,
B. the binder of the high active layer in bottom obtained is brushed in the way of brushing or spraying high-purity made from step (1)
On layer, it is rear using spread painting in the way of mesh number is spread to crucible bottom for the efficient sand of 50 mesh, form high active layer；
(3) silicon nitride release layer sprays
Silicon nitride release layer is made of silicon nitride, pure water and silica solution, in mass ratio meter silicon nitride: pure water: silica solution=1:
2.5:0.5；
Silicon nitride in silicon nitride release layer is by Ah method's Phase Proportion >=95%, tenor≤1ppm specification silicon nitride and A Fa
50%, tenor≤3ppm specification silicon nitride mixes Phase Proportion according to mass ratio 1:1；
The mixture of silicon nitride release layer is sprayed into inner surface of crucible in the way of spraying, 80 DEG C of spraying temperature, spraying is enclosed
Number 20 encloses；
(4) it charges
Loading stage, according to conventional charging method, first seed crystal small powder-reclaimed materials-routine block step, by weight in 0.8T
Silicon material be charged in crucible；
(5) ingot casting
Silicon material is packed into polycrystalline furnace according to old process, by normal occlusion stove evacuation after dress heat preservation strip, is heated to 1560 DEG C, so that
After silicon material is melted completely, by controlling the top central region temperature (TC1) and heat-insulation cage aperture of ingot casting, into crystal growing stage,
Until long brilliant completion.
In the present embodiment, Fe content≤1ppm, solid concentration 30% in silica solution.
Embodiment 2
A kind of preparation method of the efficient silicon ingot of fine melt of low metal pollution provided in this embodiment, including following below scheme: crucible bottom
The production of high-purity layer of portion, the high active layer production in bottom, the spraying of silicon nitride release layer, charging, ingot casting, in which:
(1) high-purity layer of crucible bottom production
The tekite sand collocation of high purity crystalline sand of the tenor no more than 2ppm and tenor no more than 5ppm is mixed
It closes, according to quality than high purity crystalline sand: tekite sand=5:5 is then milled to the high purity quartz slurry solution of partial size 10um, institute
The high purity quartz slurry solution solid phase ratio obtained is 40%；
The high purity quartz slurry solution of acquisition is brushed using the method brushed in crucible surface, every crucible high purity quartz slurry
Solution usage in 1000g, after be put into tunnel kiln drying, drying temperature is 60 DEG C, and drying time 2h then takes out placement
To room temperature, high-purity layer is formed in crucible bottom；
(2) the high active layer production in bottom
A. high purity quartz obtained in step (1) is starched into solution, is diluted using silica solution as the bonding of the high active layer in bottom
Agent, wherein meter high purity quartz in mass ratio starches solution: silica solution=3:7,
B. the binder of the high active layer in bottom obtained is brushed in the way of brushing or spraying high-purity made from step (1)
On layer, it is rear using spread painting in the way of mesh number is spread to crucible bottom for the efficient sand of 80 mesh, form high active layer；
(3) silicon nitride release layer sprays
Silicon nitride release layer is made of silicon nitride, pure water and silica solution, in mass ratio meter silicon nitride: pure water: silica solution=1:
3.5:0.5；When the crucible of use is the G6 crucible having a size of 1060*1060*540mm, silicon nitride release layer sprays in step (3)
Silicon nitride dosage is controlled in 900g in silicon nitride release layer when painting；
Silicon nitride in silicon nitride release layer is by Ah method's Phase Proportion >=95%, tenor≤1ppm specification silicon nitride and A Fa
60%, tenor≤3ppm specification silicon nitride mixes Phase Proportion according to mass ratio 2:1；
The mixture of silicon nitride release layer is sprayed into inner surface of crucible in the way of spraying, 95 DEG C of spraying temperature, spraying is enclosed
Number 26 encloses；
(4) it charges
Loading stage, according to conventional charging method, first seed crystal small powder-reclaimed materials-routine block step, by weight in 0.9T
Silicon material be charged in crucible；
(5) ingot casting
G6 silicon material is packed into G6 polycrystalline furnace according to old process, by normal occlusion stove evacuation after dress heat preservation strip, is heated to 1560 DEG C,
So that after silicon material is melted completely, by controlling the top central region temperature (TC1) and heat-insulation cage aperture of ingot casting, into long brilliant rank
Section, until long brilliant completion.
In the present embodiment, Fe content≤1ppm, solid concentration 30% in silica solution.
Embodiment 3
A kind of preparation method of the efficient silicon ingot of fine melt of low metal pollution provided in this embodiment, including following below scheme: crucible bottom
The production of high-purity layer of portion, the high active layer production in bottom, the spraying of silicon nitride release layer, charging, ingot casting, in which:
(1) high-purity layer of crucible bottom production
The tekite sand collocation of high purity crystalline sand of the tenor no more than 2ppm and tenor no more than 5ppm is mixed
It closes, according to quality than high purity crystalline sand: tekite sand=5:7 is then milled to the high purity quartz slurry solution of partial size 8um, gained
High purity quartz slurry solution solid phase ratio 35%；
The high purity quartz slurry solution of acquisition is brushed using the method brushed in crucible surface, every crucible high purity quartz slurry
Solution usage in 900g, after be put into tunnel kiln drying, drying temperature is 55 DEG C, and drying time 1.5h then takes out placement
To room temperature, high-purity layer is formed in crucible bottom；
(2) the high active layer production in bottom
A. high purity quartz obtained in step (1) is starched into solution, is diluted using silica solution as the bonding of the high active layer in bottom
Agent, wherein meter high purity quartz in mass ratio starches solution: silica solution=3:7,
B. the binder of the high active layer in bottom obtained is brushed in the way of brushing or spraying high-purity made from step (1)
On layer, it is rear using spread painting in the way of mesh number is spread to crucible bottom for the efficient sand of 70 mesh, form high active layer；
(3) silicon nitride release layer sprays
Silicon nitride release layer is made of silicon nitride, pure water and silica solution, in mass ratio meter silicon nitride: pure water: silica solution=1:3:
0.5；When the crucible of use is the G6 crucible having a size of 1060*1060*540mm, when silicon nitride release layer sprays in step (3)
The control of silicon nitride dosage is in 800g in silicon nitride release layer；
Silicon nitride in silicon nitride release layer is by Ah method's Phase Proportion >=95%, tenor≤1ppm specification silicon nitride and A Fa
55%, tenor≤3ppm specification silicon nitride mixes Phase Proportion according to mass ratio 1.5:1；
The mixture of silicon nitride release layer is sprayed into inner surface of crucible in the way of spraying, 90 DEG C of spraying temperature, spraying is enclosed
Number 24 encloses；
(4) it charges
Loading stage, according to conventional charging method, first seed crystal small powder-reclaimed materials-routine block step exists weight
The silicon material of 0.85T is charged in crucible；
(5) ingot casting
G6 silicon material is packed into G6 polycrystalline furnace according to old process, by normal occlusion stove evacuation after dress heat preservation strip, is heated to 1560 DEG C,
So that after silicon material is melted completely, by controlling the top central region temperature (TC1) and heat-insulation cage aperture of ingot casting, into long brilliant rank
Section, until long brilliant completion.
In the present embodiment, Fe content≤1ppm, solid concentration 30% in silica solution.
In the present embodiment, charging and ingot casting are implemented by common process in the prior art, control the top central region of ingot casting
Temperature (TC1) and heat-insulation cage aperture also press common process implementation in the prior art.
Fig. 1 is few sub- detection figure of silicon ingot before improving in the prior art, and Fig. 2 is the few son of silicon ingot obtained after the present invention improves
Detection figure, two figures in proportion, are placed in parallel to draw a dotted line up and down and compare, and silicon ingot bottom is less than in the embodiment of the present invention
The width of 4us reduces 10mm or so than prior art silicon ingot.
In addition to the implementation, the present invention can also have other embodiments.It is all to use equivalent substitution or equivalent transformation shape
At technical solution, fall within the scope of protection required by the present invention.
Claims (3)
1. a kind of preparation method of the efficient silicon ingot of fine melt of low metal pollution, which is characterized in that including following below scheme: crucible bottom
The high active layer production in high-purity layer of production-bottom-silicon nitride release layer spraying-charging-ingot casting, in which:
(1) high-purity layer of crucible bottom production
Tekite sand collocation of high purity crystalline sand of the tenor no more than 2ppm with tenor no more than 5ppm mixes,
According to quality than high purity crystalline sand: tekite sand=3:7-5:5 is then milled to the high purity quartz slurry solution of partial size 5-10um,
Resulting high purity quartz slurry solution solid phase ratio is in 30%-40%；
The high purity quartz slurry solution of acquisition is brushed using the method brushed in crucible surface, every crucible high purity quartz slurry is molten
Liquid dosage in 800-1000g, after be put into tunnel kiln drying, drying temperature is 50-60 DEG C, then drying time 1-2h takes
It is placed out to room temperature, forms high-purity layer in crucible bottom；
(2) the high active layer production in bottom
A. high purity quartz obtained in step (1) is starched into solution, is diluted using silica solution as the bonding of the high active layer in bottom
Agent, wherein meter high purity quartz in mass ratio starches solution: silica solution=3:7,
B. the binder of the high active layer in bottom obtained is brushed in the way of brushing or spraying high-purity made from step (1)
On layer, it is rear using spread painting in the way of mesh number is spread to crucible bottom for the efficient sand of 50-80 mesh, form high active layer；
(3) silicon nitride release layer sprays
Silicon nitride release layer is made of silicon nitride, pure water and silica solution, in mass ratio meter silicon nitride: pure water: silica solution=1:
2.5-3.5:0.5；
Silicon nitride in silicon nitride release layer is by Ah method's Phase Proportion >=95%, tenor≤1ppm specification silicon nitride and A Fa
Phase Proportion is mixed in 50%-60%, tenor≤3ppm specification silicon nitride according to mass ratio 1:1-2:1；
The mixture of silicon nitride release layer is sprayed into inner surface of crucible in the way of spraying, 80-95 DEG C of spraying temperature, is sprayed
Enclose number 20-26 circle；
(4) it charges
Loading stage, according to conventional charging method, silicon material is charged to by first seed crystal small powder-reclaimed materials-routine block step
In crucible；
(5) ingot casting
Silicon material is packed into polycrystalline furnace according to old process, by normal occlusion stove evacuation after dress heat preservation strip, is heated to 1560 DEG C, so that
After silicon material is melted completely, by controlling the top central region temperature (TC1) and heat-insulation cage aperture of ingot casting, into crystal growing stage,
Until long brilliant completion.
2. the preparation method of the efficient silicon ingot of fine melt of low metal pollution according to claim 1, it is characterised in that: the silicon
Fe content≤1ppm, solid concentration 30% in colloidal sol.
3. the preparation method of the efficient silicon ingot of fine melt of low metal pollution according to claim 1, it is characterised in that: use
When crucible is the G6 crucible having a size of 1060*1060*540mm, silicon nitride is demoulded when silicon nitride release layer sprays in step (3)
The control of silicon nitride dosage is in 800-900g in layer.
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| CN112064112A (en) * | 2020-09-15 | 2020-12-11 | 晶科能源有限公司 | Crucible, preparation method thereof and device for preparing silicon crystal |
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