CN107338474A - One kind reduces polycrystalline silicon ingot casting oxygen content method - Google Patents
One kind reduces polycrystalline silicon ingot casting oxygen content method Download PDFInfo
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- CN107338474A CN107338474A CN201710657888.XA CN201710657888A CN107338474A CN 107338474 A CN107338474 A CN 107338474A CN 201710657888 A CN201710657888 A CN 201710657888A CN 107338474 A CN107338474 A CN 107338474A
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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
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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
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/02—Heat treatment
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Abstract
The present invention relates to one kind to reduce polycrystalline silicon ingot casting oxygen content method, wherein, comprise the following steps：Spray treatment is carried out to a crucible, input mixing silicon material in the crucible completed to spraying；Heating is carried out until the mixing silicon material is in molten condition after vacuumize process will be carried out after the crucible one ingot furnace of placement for being filled with the mixing silicon material；Argon gas is passed through with default air velocity into the ingot furnace and the air pressure in the ingot furnace is reduced to after the first air pressure and proceeds by long brilliant operation；Solidification is oriented to the mixing silicon material until completing long brilliant process after the melting temperature of the mixing silicon material is down to the crystallization temperature of the polycrystalline silicon ingot casting；Treat to be annealed and cooled down successively to obtain the polycrystalline silicon ingot casting after long brilliant completion.Reduction polycrystalline silicon ingot casting oxygen content method proposed by the present invention, can be prepared the lower polycrystalline cast ingot of oxygen content, meet practical application request.
Description
Technical field
It is more particularly to a kind of to reduce polycrystalline silicon ingot casting oxygen content method the present invention relates to technical field of crystal growth.
Background technology
Recently come, photovoltaic generation as a kind of new energy conversion means, due to the advantages that its is renewable, cleaning by
Gradually turn into the energy generation technologies of main flow, increasingly paid much attention to by researcher, have in the energy field in future
There is great development potentiality.
Restricting the key factor of photovoltaic industry development at present includes two aspects：One is that electricity conversion is low, secondly
It is higher for the cost of manufacture of solar cell.It is well known that photovoltaic silicon wafer is the basic material for producing solar cell and component
Material, the polysilicon purity for producing photovoltaic silicon wafer must be more than 6N levels, and otherwise the performance of photovoltaic cell is by by very big
Negative effect.In recent years, the production technology of polysilicon chip has the progress of highly significant, specifically, polycrystalline cast ingot technology from
G5 (5 × 5=25 silicon side) is arrived in G4 (each silicon ingot weighs about 270 kilograms, can cut 4 × 4=16 silicon side) progress, until arriving G6 (6
× 6=36 silicon side).At the same time, the unit volume of the polycrystalline silicon ingot casting obtained by producing incrementally increases, and yield rate also obtains
Certain increase, and the manufacturing cost of polycrystalline silicon ingot casting also gradually reducing.
However, in the actual manufacturing process of polycrystalline cast ingot, due to OXO products caused by silicon liquid and silica crucible reaction
It is difficult to discharge in time, easily dissolves or be deposited in polycrystal silicon ingot, causes the oxygen content during ingot casting to raise and then cause too
The problem of photo attenuation occurs for positive energy battery, reduce the efficiency of solar cell.
The content of the invention
Based on this, it is an object of the invention to propose that one kind can effectively reduce oxygen in polycrystalline cast ingot in actual applications to contain
The preparation method of amount, to improve the quality of product, meet practical application request.
The present invention proposes a kind of reduction polycrystalline silicon ingot casting oxygen content method, wherein, comprise the following steps：
Spray treatment is carried out to a crucible, input mixing silicon material in the crucible completed to spraying；
Heated after vacuumize process will be carried out after the crucible one ingot furnace of placement for being filled with the mixing silicon material
Until the mixing silicon material is in molten condition；
Argon gas is passed through with default air velocity into the ingot furnace and the air pressure in the ingot furnace is reduced to first
Long brilliant operation is proceeded by after air pressure；
To the mixing silicon material after the melting temperature of the mixing silicon material is down to the crystallization temperature of the polycrystalline silicon ingot casting
Solidification is oriented until completing long brilliant process；
Treat to be annealed and cooled down successively to obtain the polycrystalline silicon ingot casting after long brilliant completion.
Reduction polycrystalline silicon ingot casting oxygen content method proposed by the present invention, after the mixing silicon material in crucible is in molten condition
Phase, argon gas is passed through with default air velocity into ingot furnace and the air pressure in ingot furnace is reduced to the first air pressure, this method can
To accelerate the flowing velocity of ingot casting furnace gas so that caused oxygenatedchemicals to be discharged in time, so as to finally reduce polysilicon
Oxygen content in ingot casting, meet technique productions requirement.Reduction polycrystalline silicon ingot casting oxygen content method proposed by the present invention, can be prepared
The lower polycrystalline cast ingot of oxygen content is obtained, meets practical application request.
The reduction polycrystalline silicon ingot casting oxygen content method, wherein, the default air velocity is 35.0~35.5slpm.
The reduction polycrystalline silicon ingot casting oxygen content method, wherein, first air pressure is 300-400mbar.
The reduction polycrystalline silicon ingot casting oxygen content method, wherein, the crucible is a silica crucible, described that a crucible is entered
The step of row spray treatment, includes：
It is configured to spray the coating spraying liquid of the crucible；
The coating spraying liquid is homogeneously applied on the inner surface of the crucible；
The crucible for spraying completion is subjected to drying and processing in a drying plant.
It is described reduction polycrystalline silicon ingot casting oxygen content method, wherein, the coating spraying liquid include silicon nitride powder, Ludox with
And high purity water, corresponding mass percent are respectively 30%, 10% and 60%.
The reduction polycrystalline silicon ingot casting oxygen content method, wherein, the particle diameter of the silicon nitride powder is 1.1~2.0um, described
The viscosity of Ludox is 5.0~7.0mPa.S, and the pH value of the Ludox is 8.5~9.8.
The reduction polycrystalline silicon ingot casting oxygen content method, wherein, the pH value of the high purity water is 6.8~7.0, and electrical conductivity is
0.1~0.6us/cm.
The reduction polycrystalline silicon ingot casting oxygen content method, wherein, the mixing silicon material includes virgin polycrystalline silicon, expect end to end,
Single polycrystalline flaw-piece, broken silicon wafers, circulation silico briquette and foundry alloy, the mass fraction of the virgin polycrystalline silicon is 57%~65%, institute
It is 13%~15% to state the mass fraction expected end to end, and the mass fraction of single polycrystalline flaw-piece is 11%~14%, the broken silicon
The mass fraction of piece is 5%~6%, and the mass fraction of the circulation silico briquette is 3%~5%, the mass fraction of the foundry alloy
For 0.01%~0.05%.
The reduction polycrystalline silicon ingot casting oxygen content method, wherein, the crucible that the mixing silicon material will be filled with
Place and carry out heating after vacuumize process is carried out after an ingot furnace until the mixing silicon material includes the step of being in molten condition：
The ingot furnace is carried out to vacuumize 1~1.5h；
3~4h of heating is carried out to the mixing silicon material until the temperature of the mixing silicon material reaches melting temperature, wherein institute
Melting temperature is stated as 1530~1550 DEG C.
The reduction polycrystalline silicon ingot casting oxygen content method, wherein, it is described treat to carry out successively after long brilliant complete annealing with it is cold
But to obtain polycrystalline silicon ingot casting the step of includes：
Wait the 9~9.5h that annealed after growing brilliant complete within the temperature range of 1360~750 DEG C；
8.5~9h of natural cooling is cast with obtaining the polysilicon within the temperature range of 750~370 DEG C after annealing completion
Ingot.
The additional aspect and advantage of the present invention will be set forth in part in the description, and will partly become from the following description
Obtain substantially, or recognized by the practice of the present invention.
Brief description of the drawings
Fig. 1 is the flow chart of the reduction polycrystalline silicon ingot casting oxygen content method in the embodiment of the present invention one.
Fig. 2 is argon flow amount control signal in the reduction polycrystalline silicon ingot casting oxygen content method that the embodiment of the present invention one proposes
Figure；
Fig. 3 is furnace pressure control signal in the reduction polycrystalline silicon ingot casting oxygen content method that the embodiment of the present invention one proposes
Figure.
Embodiment
For the ease of understanding the present invention, the present invention is described more fully below with reference to relevant drawings.In accompanying drawing
Give the preferred embodiment of the present invention.But the present invention can realize in many different forms, however it is not limited to this paper institutes
The embodiment of description.On the contrary, the purpose for providing these embodiments is made to the disclosure more thorough and comprehensive.
Unless otherwise defined, all of technologies and scientific terms used here by the article is with belonging to technical field of the invention
The implication that technical staff is generally understood that is identical.Term used in the description of the invention herein is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.Term as used herein " and/or " include one or more phases
The arbitrary and all combination of the Listed Items of pass.
Embodiment one
Fig. 1 to Fig. 3 is referred to, for the reduction polycrystalline silicon ingot casting oxygen content method in first embodiment of the invention, including
Step S101-S105.
Step S101, spray treatment is carried out to a crucible, input mixing silicon material in the crucible completed to spraying.
Wherein, the crucible is a silica crucible, when carrying out spray treatment to the crucible, needs to be configured to spray first
Apply the coating spraying liquid of the crucible；Then the coating spraying liquid is homogeneously applied on the inner surface of the crucible；Most
The crucible for spraying completion is subjected to drying and processing in a drying plant afterwards.
Specifically, the coating spraying liquid that configuration obtains includes silicon nitride powder, Ludox and high purity water, wherein described
Coating spraying liquid includes silicon nitride powder, Ludox and high purity water, corresponding mass percent be respectively 30%, 10% and
60%.
For the silicon nitride powder, the particle diameter of selected silicon nitride powder is 1.1~2.0um, in the Ludox
SiO2Solid content be 20~30%, corresponding particle diameter is 10~50nm, and the viscosity of the Ludox is 5.0~7.0mPa.S,
Corresponding pH value is 8.5~9.8.In addition, for the high purity water, the pH value of the high purity water is 6.8~7.0, electrical conductivity
For 0.1~0.6us/cm.
After spraying is completed, the input mixing silicon material into the crucible.Wherein, the mixing silicon material includes primary polycrystalline
Silicon, material, single polycrystalline flaw-piece, broken silicon wafers, circulation silico briquette and foundry alloy end to end, the mass fraction of the virgin polycrystalline silicon is 57%
~65%, the mass fraction expected end to end is 13%~15%, and the mass fraction of single polycrystalline flaw-piece is 11%~14%,
The mass fraction of the broken silicon wafers is 5%~6%, and the mass fraction of the circulation silico briquette is 3%~5%, the foundry alloy
Mass fraction is 0.01%~0.05%.
Step S102, after vacuumize process is carried out after the crucible one ingot furnace of placement for being filled with the mixing silicon material
Heating is carried out until the mixing silicon material is in molten condition.
As described above, after filling the mixing silicon material in the crucible, the crucible for being filled with mixing silicon material is put
The ingot furnace is carried out to vacuumize 1~1.5h after entering in an ingot furnace, waits to enter the mixing silicon material after vacuumizing completion
Row 3~4h of heating is until the temperature of the mixing silicon material reaches melting temperature, wherein the melting temperature is 1530~1550 DEG C.
Step S103, argon gas is passed through and by the air pressure drop in the ingot furnace with default air velocity into the ingot furnace
Long brilliant operation is proceeded by after as little as the first air pressure.
In above-mentioned steps, when the mixing silicon material in the crucible is in the molten condition later stage, with 35.0~
35.5slpm (ratio of corresponding argon gas is 70%) default air velocity is passed through argon gas (shown in Fig. 2) into the ingot furnace,
And the air pressure in the ingot furnace is reduced to 300-400mbar (shown in Fig. 3), long brilliant operation is proceeded by the present context.
Step S104, to described after the melting temperature of the mixing silicon material is down to the crystallization temperature of the polycrystalline silicon ingot casting
Mixing silicon material is oriented solidification until completing long brilliant process.
In crystal growing process, it is necessary to by it is described mixing silicon material from melting temperature be gradually decreased to crystallization temperature after again to this
Mixing silicon material is oriented solidification (crystal pulling) until completing whole brilliant processes of length, and wherein the crystallization temperature is 1430~1450
℃。
Step S105, treat to be annealed and cooled down successively to obtain the polycrystalline silicon ingot casting after long brilliant completion.
In this step, 9~9.5h of annealing is carried out under 1360~750 DEG C of temperature range after long brilliant completion；Treat
8.5~9h of natural cooling finally gives the polycrystalline silicon ingot casting within the temperature range of 750~370 DEG C after annealing completion.
Reduction polycrystalline silicon ingot casting oxygen content method proposed by the present invention, after the mixing silicon material in crucible is in molten condition
Phase, argon gas is passed through using 35.0~35.5slpm (correspondingly the ratio of argon gas is 70%) default air velocity into ingot furnace and incited somebody to action
Air pressure in ingot furnace is reduced to 300-400mbar, and this method can accelerate the flowing velocity of ingot casting furnace gas that will produce
Oxygenatedchemicals discharge in time, so as to finally reduce polycrystalline silicon ingot casting in oxygen content, meet technique productions requirement.This hair
The reduction polycrystalline silicon ingot casting oxygen content method of bright proposition, can be prepared the lower polycrystalline cast ingot of oxygen content, meet reality
Application demand.
Embodiment two
Spray treatment is carried out to a crucible first, input mixing silicon material in the crucible completed to spraying.Specifically, first
Configure coating spraying liquid；Then coating spraying liquid is homogeneously applied on the inner surface of crucible；Crucible is entered after the completion of spraying
Row drying and processing.Specifically, silicon nitride powder, Ludox and matter corresponding to high purity water difference in the coating spraying liquid that configuration obtains
It is respectively 30%, 10% and 60% to measure percentage.
Wherein, the particle diameter of silicon nitride powder is 1.1um, SiO in Ludox2Solid content be 20%, corresponding particle diameter is
15nm, the viscosity of Ludox is 5.0mPa.S, and corresponding pH value is 8.5.In addition, the pH value of high purity water is 6.8, electrical conductivity is
0.1us/cm。
In addition, add mixing silicon material include virgin polycrystalline silicon, end to end material, single polycrystalline flaw-piece, broken silicon wafers, circulate silico briquette with
And foundry alloy, the mass fraction of virgin polycrystalline silicon is 63%, and the mass fraction expected end to end is 13%, the quality point of single polycrystalline flaw-piece
Number is 14%, and the mass fraction of broken silicon wafers is 6%, and the mass fraction for circulating silico briquette is 3.95%, and the mass fraction of foundry alloy is
0.05%.
Then, the ingot furnace for being filled with mixing silicon material is carried out to carry out heating 3h until mixing silicon material is in after vacuumizing 1h
Molten condition, the temperature of corresponding molten condition is 1530 DEG C.
Further, argon gas is passed through and by the air pressure in ingot furnace with 35.0slpm default air velocity into ingot furnace
It is reduced to 300mbar and proceeds by long brilliant operation afterwards.
And then, to described mixed after the melting temperature of the mixing silicon material is down to the crystallization temperature of the polycrystalline silicon ingot casting
Close silicon material and be oriented solidification until completing long brilliant process.Wherein the crystallization temperature is 1430 DEG C.
Finally, treat to carry out annealing 9h under 1360 DEG C of temperature range after long brilliant completion, 750 after completion to be annealed
Natural cooling 8.5h finally gives the polycrystalline silicon ingot casting within the temperature range of DEG C.
Embodiment three
Spray treatment is carried out to a crucible first, input mixing silicon material in the crucible completed to spraying.Specifically, first
Configure coating spraying liquid；Then coating spraying liquid is homogeneously applied on the inner surface of crucible；Crucible is entered after the completion of spraying
Row drying and processing.Specifically, silicon nitride powder, Ludox and matter corresponding to high purity water difference in the coating spraying liquid that configuration obtains
It is respectively 30%, 10% and 60% to measure percentage.
Wherein, the particle diameter of silicon nitride powder is 2.0um, SiO in Ludox2Solid content be 30%, corresponding particle diameter is
50nm, the viscosity of Ludox is 7.0mPa.S, and corresponding pH value is 9.8.In addition, the pH value of high purity water is 7.0, electrical conductivity is
0.6us/cm。
In addition, add mixing silicon material include virgin polycrystalline silicon, end to end material, single polycrystalline flaw-piece, broken silicon wafers, circulate silico briquette with
And foundry alloy, the mass fraction of virgin polycrystalline silicon is 65%, and the mass fraction expected end to end is 13%, the quality point of single polycrystalline flaw-piece
Number is 11%, and the mass fraction of broken silicon wafers is 6%, and the mass fraction for circulating silico briquette is 4.99%, and the mass fraction of foundry alloy is
0.01%.
Then, the ingot furnace for being filled with mixing silicon material is carried out to carry out heating 4h until at mixing silicon material after vacuumizing 1.5h
In molten condition, the temperature of corresponding molten condition is 1550 DEG C.
Further, argon gas is passed through and by the air pressure in ingot furnace with 35.5slpm default air velocity into ingot furnace
It is reduced to 400mbar and proceeds by long brilliant operation afterwards.
And then, to described mixed after the melting temperature of the mixing silicon material is down to the crystallization temperature of the polycrystalline silicon ingot casting
Close silicon material and be oriented solidification until completing long brilliant process.Wherein the crystallization temperature is 1450 DEG C.
Finally, treat to carry out annealing 9.5h under 1360 DEG C of temperature range after long brilliant completion, exist after completion to be annealed
Natural cooling 9h finally gives the polycrystalline silicon ingot casting within the temperature range of 750 DEG C.
Example IV
Spray treatment is carried out to a crucible first, input mixing silicon material in the crucible completed to spraying.Specifically, first
Configure coating spraying liquid；Then coating spraying liquid is homogeneously applied on the inner surface of crucible；Crucible is entered after the completion of spraying
Row drying and processing.Specifically, silicon nitride powder, Ludox and matter corresponding to high purity water difference in the coating spraying liquid that configuration obtains
It is respectively 30%, 10% and 60% to measure percentage.
Wherein, the particle diameter of silicon nitride powder is 1.6um, SiO in Ludox2Solid content be 25%, corresponding particle diameter is
25nm, the viscosity of Ludox is 6.0mPa.S, and corresponding pH value is 9.2.In addition, the pH value of high purity water is 6.9, electrical conductivity is
0.4us/cm。
In addition, add mixing silicon material include virgin polycrystalline silicon, end to end material, single polycrystalline flaw-piece, broken silicon wafers, circulate silico briquette with
And foundry alloy, the mass fraction of virgin polycrystalline silicon is 63%, and the mass fraction expected end to end is 14%, the quality point of single polycrystalline flaw-piece
Number is 12.5%, and the mass fraction of broken silicon wafers is 6%, and the mass fraction for circulating silico briquette is 4.47%, the mass fraction of foundry alloy
For 0.03%.
Then, the ingot furnace for being filled with mixing silicon material is carried out to carry out heating 3.5h until mixing silicon after vacuumizing 1.25h
Material is in molten condition, and the temperature of corresponding molten condition is 1545 DEG C.
Further, argon gas is passed through and by the gas in ingot furnace with 35.25slpm default air velocity into ingot furnace
Long brilliant operation is proceeded by after pressure drop as little as 350mbar.
And then, to described mixed after the melting temperature of the mixing silicon material is down to the crystallization temperature of the polycrystalline silicon ingot casting
Close silicon material and be oriented solidification until completing long brilliant process.Wherein the crystallization temperature is 1440 DEG C.
Finally, treat to carry out annealing 9.25h under 1360 DEG C of temperature range after long brilliant completion, exist after completion to be annealed
Natural cooling 8.75h finally gives the polycrystalline silicon ingot casting within the temperature range of 750 DEG C.
Reduction polycrystalline silicon ingot casting oxygen content method proposed by the present invention, after the mixing silicon material in crucible is in molten condition
Phase, argon gas is passed through with 35.0~35.5slpm default air velocity into ingot furnace and is adjusted to the air pressure in ingot furnace
300-400mbar, this method can accelerate the flowing velocity of ingot casting furnace gas so that caused oxygenatedchemicals to be arranged in time
Go out, so as to finally reduce the oxygen content in polycrystalline silicon ingot casting, meet technique productions requirement.Reduction polysilicon casting proposed by the present invention
Ingot oxygen content method, the lower polycrystalline cast ingot of oxygen content can be prepared, meet practical application request.
To sum up, the polycrystalline cast ingot obtained by the method in above-described embodiment one to four, its oxygen content by routine 6.0~
6.5×1017cm-3It is reduced to 4.2~4.5 × 1017cm-3, the oxygen in polycrystalline cast ingot can effectively be reduced using the preparation method and contained
Amount, due to reducing the oxygen content in polycrystalline cast ingot so that photo attenuation has also decreased 1.12%, and then causes battery effect
Rate improves 0.021%, meets practical application request.
Embodiment described above only expresses the several embodiments of the present invention, and its description is more specific and detailed, but simultaneously
Therefore the limitation to the scope of the claims of the present invention can not be interpreted as.It should be pointed out that for one of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the guarantor of the present invention
Protect scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (10)
1. one kind reduces polycrystalline silicon ingot casting oxygen content method, it is characterised in that comprises the following steps：
Spray treatment is carried out to a crucible, input mixing silicon material in the crucible completed to spraying；
Will be filled with it is described mixing silicon material the crucible place an ingot furnace after carry out vacuumize process after carry out heating until
The mixing silicon material is in molten condition；
Argon gas is passed through with default air velocity into the ingot furnace and the air pressure in the ingot furnace is reduced to the first air pressure
After proceed by long brilliant operation；
The mixing silicon material is carried out after the melting temperature of the mixing silicon material is down to the crystallization temperature of the polycrystalline silicon ingot casting
Directional solidification is until complete long brilliant process；
Treat to be annealed and cooled down successively to obtain the polycrystalline silicon ingot casting after long brilliant completion.
2. reduction polycrystalline silicon ingot casting oxygen content method according to claim 1, it is characterised in that the default air velocity
For 35.0~35.5slpm.
3. reduction polycrystalline silicon ingot casting oxygen content method according to claim 1, it is characterised in that first air pressure is
300-400mbar。
4. reduction polycrystalline silicon ingot casting oxygen content method according to claim 1, it is characterised in that the crucible is a quartz
Crucible, described the step of carrying out spray treatment to a crucible, include：
It is configured to spray the coating spraying liquid of the crucible；
The coating spraying liquid is homogeneously applied on the inner surface of the crucible；
The crucible for spraying completion is subjected to drying and processing in a drying plant.
5. reduction polycrystalline silicon ingot casting oxygen content method according to claim 4, it is characterised in that the coating spraying liquid bag
Silicon nitride powder, Ludox and high purity water are included, corresponding mass percent is respectively 30%, 10% and 60%.
6. reduction polycrystalline silicon ingot casting oxygen content method according to claim 5, it is characterised in that the grain of the silicon nitride powder
Footpath is 1.1~2.0um, and the viscosity of the Ludox is 5.0~7.0mPa.S, and the pH value of the Ludox is 8.5~9.8.
7. reduction polycrystalline silicon ingot casting oxygen content method according to claim 5, it is characterised in that the pH value of the high purity water
For 6.8~7.0, electrical conductivity is 0.1~0.6us/cm.
8. reduction polycrystalline silicon ingot casting oxygen content method according to claim 1, it is characterised in that the mixing silicon material includes
Virgin polycrystalline silicon, material, single polycrystalline flaw-piece, broken silicon wafers, circulation silico briquette and foundry alloy, the quality of the virgin polycrystalline silicon are divided end to end
Number is 57%~65%, and the mass fraction expected end to end is 13%~15%, and the mass fraction of single polycrystalline flaw-piece is
11%~14%, the mass fraction of the broken silicon wafers is 5%~6%, and the mass fraction of the circulation silico briquette is 3%~5%, institute
The mass fraction for stating foundry alloy is 0.01%~0.05%.
9. reduction polycrystalline silicon ingot casting oxygen content method according to claim 1, it is characterised in that it is described will be filled with it is described
Heating is carried out after carrying out vacuumize process after the crucible one ingot furnace of placement of mixing silicon material until the mixing silicon material is in
The step of molten condition, includes：
The ingot furnace is carried out to vacuumize 1~1.5h；
3~4h of heating is carried out to the mixing silicon material until the temperature of the mixing silicon material reaches melting temperature, wherein described molten
Melt temperature as 1530~1550 DEG C.
10. reduction polycrystalline silicon ingot casting oxygen content method according to claim 1, it is characterised in that described to treat long brilliant completion
The step of being annealed and cooled down to obtain the polycrystalline silicon ingot casting successively afterwards includes：
Wait the 9~9.5h that annealed after growing brilliant complete within the temperature range of 1360~750 DEG C；
Annealing complete after within the temperature range of 750~370 DEG C 8.5~9h of natural cooling to obtain the polycrystalline silicon ingot casting.
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| CN108486651A (en) * | 2018-06-28 | 2018-09-04 | 英利能源（中国）有限公司 | The preparation method and polycrystal silicon ingot of polycrystal silicon ingot |
| CN109853035A (en) * | 2019-04-19 | 2019-06-07 | 晶科能源有限公司 | Crucible and the polycrystalline silicon ingot casting method for using the crucible |
| CN112891973A (en) * | 2021-01-15 | 2021-06-04 | 中国科学院上海应用物理研究所 | Method for reducing oxygen content in halide molten salt |
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