CN108531984A - A method of reducing ingot casting carbon oxygen content for polycrystalline silicon ingot or purifying furnace - Google Patents
A method of reducing ingot casting carbon oxygen content for polycrystalline silicon ingot or purifying furnace Download PDFInfo
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- CN108531984A CN108531984A CN201810598214.1A CN201810598214A CN108531984A CN 108531984 A CN108531984 A CN 108531984A CN 201810598214 A CN201810598214 A CN 201810598214A CN 108531984 A CN108531984 A CN 108531984A
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- polycrystalline silicon
- ingot casting
- oxygen content
- ingot
- backplate
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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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- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
A method of ingot casting carbon oxygen content being reduced for polycrystalline silicon ingot or purifying furnace, this approach includes the following steps：（1）Spraying silicon nitride slurry is carried out as release layer to silica crucible, then it feeds and opens foraminate backplate, backplate size a length of 500mm 1200mm, a height of 300mm 600mm in the setting of crucible surrounding, it is positioned on graphite bottom plate, is put into material in orientation ingot furnace with fork truck；（2）Stove operation is closed, is heated to being passed through argon gas at 800 900 DEG C after vacuumize process, between setting air inflow is 50% 90%, 1550 DEG C are continuously heating to, until silicon material is in molten condition；（3）Then it opens heat-insulation cage and reduces setting temperature, solidification is oriented to mixing silicon material after the melting temperature of silicon material is down to the crystallization temperature of polycrystalline silicon ingot casting until completing long brilliant process；（4）It waits for that long brilliant completion carries out annealing and obtains polycrystalline silicon ingot casting with cooling successively later, and takes the print progress carbon oxygen content test at crucible bottom 50mm of center silico briquette.
Description
Technical field
The present invention relates to a kind of methods reducing ingot casting carbon oxygen content for polycrystalline silicon ingot or purifying furnace.
Background technology
All it is currently to carry out ingot casting using directional solidification ingot furnace in the industry, has a large amount of graphite piece such as in ingot furnace：Graphite
Heater, heat-insulation cage thermal insulation board, crucible guard boards, crucible cover plate etc., under hot conditions during ingot casting, it is easy in silicon
A large amount of carbon impurities are introduced in melt, in addition also with oxygen, silica crucible etc. chemistry can occur for these graphite members under the high temperature conditions
Reaction, which generates gases, these gases such as CO, SiO, can be entered in silicon melt by internal gas flow to introduce carbon oxygen impurities；Generally
Oxygen is existed in hypersaturated state with gap state, and for ingot casting there are one the process of high temperature to low temperature, oxygen concentration is excessively high in this process
In will form Thermal donor or oxygen precipitation, become complex centre so that influence silicon ingot minority carrier life time, influence the light of cell piece
Photoelectric transformation efficiency；Carbon impurity can be used as oxygen precipitation core and form grown-in oxygen precipitates, and SiC is likely to form when carbon content is excessively high
Grain, influences the following process of silicon ingot and the quality of silicon chip.Therefore, the carbon oxygen content introduced during ingot casting is reduced to polysilicon
Ingot casting link is of great significance.
During existing ingot casting, the graphite device of furnace interior can at high temperature react generation one with silica crucible
The pernicious gases such as carbonoxide, silicon monoxide, recycle above silicon melt, it is difficult to which silicon solution, backplate, cover board is discharged, and this is integrally
System is outer, and the overlong time that pernicious gas is acted on silicon melt causes the carbon oxygen in silicon ingot to be dissolved in silicon melt by absorption
Content rises.
Invention content
Its purpose of the invention, which is that, provides a kind of method reducing ingot casting carbon oxygen content for polycrystalline silicon ingot or purifying furnace, solves
During existing ingot casting, there are pernicious gases and the overlong time of silicon melt effect to be dissolved in silicon melt by absorption
In, the problem of causing carbon oxygen content in silicon ingot to rise.
It adopts the technical scheme that achieve the above object, a method of reducing ingot casting carbon oxygen content, this method packet
Include following steps：
（1）Spraying silicon nitride slurry is carried out as release layer to silica crucible, then feed and is provided in the setting of crucible surrounding small
The backplate in hole, backplate size a length of 500mm-1200mm, a height of 300mm-600mm are positioned on graphite bottom plate, will be expected with fork truck
In input orientation ingot furnace；
（2）Close stove operation, be heated to being passed through argon gas at 800-900 DEG C after vacuumize process, setting air inflow be 50%-90% it
Between, 1550 DEG C are continuously heating to, until silicon material is in molten condition；
（3）Then it opens heat-insulation cage and reduces setting temperature, wait for that the melting temperature of silicon material is down to the crystallization temperature of polycrystalline silicon ingot casting
Solidification is oriented to mixing silicon material afterwards until completing long brilliant process；
（4）It waits for that long brilliant completion carries out annealing and obtains polycrystalline silicon ingot casting with cooling successively later, and takes center silico briquette close to crucible bottom
Print carries out carbon oxygen content test at portion 50mm.
Advantageous effect
The present invention has the following advantages compared with prior art.
It is an advantage of the invention that this method can form a stable current path from inside to outside so that in stove
Carbon impurity can not enter silicon melt by aperture, also avoid reacting between carbon and silica crucible, reduce carbon oxygen impurities
It introduces, achievees the purpose that reduce carbon oxygen content.
Description of the drawings
Below in conjunction with attached drawing, the invention will be further described.
Fig. 1 is the structural diagram of the present invention；
Fig. 2 is embodiment of the present invention schematic diagram.
Specific implementation mode
A method of ingot casting carbon oxygen content being reduced for polycrystalline silicon ingot or purifying furnace, this approach includes the following steps：
（1）Spraying silicon nitride slurry is carried out as release layer to silica crucible, then feed and is provided in the setting of crucible surrounding small
The backplate in hole, backplate size a length of 500mm-1200mm, a height of 300mm-600mm are positioned on graphite bottom plate, will be expected with fork truck
In input orientation ingot furnace；
（2）Close stove operation, be heated to being passed through argon gas at 800-900 DEG C after vacuumize process, setting air inflow be 50%-90% it
Between, 1550 DEG C are continuously heating to, until silicon material is in molten condition；
（3）Then it opens heat-insulation cage and reduces setting temperature, wait for that the melting temperature of silicon material is down to the crystallization temperature of polycrystalline silicon ingot casting
Solidification is oriented to mixing silicon material afterwards until completing long brilliant process；
（4）It waits for that long brilliant completion carries out annealing and obtains polycrystalline silicon ingot casting with cooling successively later, and takes center silico briquette close to crucible bottom
Print carries out carbon oxygen content test at portion 50mm.
The step（1）The shape that aperture is opened up on middle backplate is unlimited, and the aperture gross area opened up is in 50cm2-150cm2
Between, aperture position is in mouth of pot between backplate top.
Embodiment
A method of ingot casting carbon oxygen content being reduced for polycrystalline silicon ingot or purifying furnace, as shown in Figure 1, this method includes following step
Suddenly：
（1）Spraying silicon nitride slurry is carried out as release layer to silica crucible, then feed and is provided in the setting of crucible surrounding small
The backplate in hole, backplate size are 1088*600*25mm, have opened up the aperture of 6 diameter 20mm, the monolithic backplate aperture gross area is about
For 18.84cm2, a whole set of backplate aperture gross area is 75.36cm2, it is positioned on graphite bottom plate, material is put into orientation casting with fork truck
In ingot stove；
（2）Close stove operation, vacuumize first, be evacuated to furnace pressure be 0.01mbar after, with power heating mode（Power, which is arranged, is
65%）It is heated to being slowly introducing argon gas at 800-900 DEG C until furnace pressure stops ventilation after being 600Mbar, setting air inflow is
65%, continue to be warming up to 1550 DEG C with temperature model, until silicon material is in molten condition；
（3）Then it opens heat-insulation cage and reduces setting temperature, wait for that the melting temperature of silicon material is down to the crystallization temperature of polycrystalline silicon ingot casting
Solidification is oriented to mixing silicon material afterwards until completing long brilliant process；
（4）Wait for that carry out annealing successively after long brilliant complete obtains polycrystalline silicon ingot casting with cooling, carries out evolution detection in silicon ingot and cuts
After disconnected, silico briquette print at crucible bottom 50mm in center is taken to carry out carbon oxygen content test.
As shown in Fig. 2, described（1）The shape of the aperture opened up on middle backplate is circle, often covers the aperture that backplate opens up
The gross area is in 50cm2-150cm2Between, aperture position is in mouth of pot to backplate top centre position.
Using above-described embodiment, it is 1.85*10 to measure carbon content17Atoms/cm3, oxygen content 3.1*1017atoms/
cm3.As shown in table 1, table 1 be using this programme backplate and casting ingot method carbon oxygen content data, another column be common process with
The carbon oxygen content data of conventional the gone out ingot of backplate, it is seen that decreased significantly.
Table 1
During the melting of polycrystalline silicon casting ingot process, long crystalline substance, silicon material is heated to be molten into silicon liquid, and inlet air flow is by cover plate central position
Set between cover board and silicon liquid level, air inflow set to 30-60% by the way that casting ingot process is arranged, conventional backplate U-shaped opening compared with
Greatly, inside and outside to be difficult to form pressure difference, the stable current path flowed outward by inside can not be formed, and the carbon of stove interior is miscellaneous
Matter, which is easily entered by U-shaped opening in silicon melt, causes carbon impurity content to increase, while the generation SiO that can also react with crucible,
CO gases enter silicon melt and carbon oxygen content are caused to increase.After this programme backplate is provided with, silicon solution liquid level and cover board, backplate it
Between form a closed space, air inlet is continued by air inlet during operation, the air pressure of this enclosure space relatively it is external will greatly, and
Air-flow can only be discharged by backplate venthole, and material is thus formed a stable current path from inside to outside, carbon is miscellaneous in stove
Matter can not enter silicon melt by aperture, also avoid reacting between carbon and silica crucible, reduce the introducing of carbon oxygen impurities,
Achieve the purpose that reduce carbon oxygen content.
Claims (2)
1. a kind of method reducing ingot casting carbon oxygen content for polycrystalline silicon ingot or purifying furnace, which is characterized in that this method includes following step
Suddenly：
Spraying silicon nitride slurry is carried out as release layer to silica crucible, then feed and is opened in the setting of crucible surrounding foraminate
Backplate, backplate size a length of 500mm-1200mm, a height of 300mm-600mm are positioned on graphite bottom plate, are put into material with fork truck
It orients in ingot furnace；
Stove operation is closed, is heated to being passed through argon gas at 800-900 DEG C after vacuumize process, air inflow is set between 50%-90%, after
It is continuous to be warming up to 1550 DEG C, until silicon material is in molten condition；
Then it opens heat-insulation cage and reduces setting temperature, it is right after the melting temperature of silicon material is down to the crystallization temperature of polycrystalline silicon ingot casting
Mixing silicon material is oriented solidification until completing long brilliant process；
It waits for that long brilliant completion carries out annealing and obtains polycrystalline silicon ingot casting with cooling successively later, and takes center silico briquette close to crucible bottom
Print carries out carbon oxygen content test at 50mm.
2. a kind of method reducing ingot casting carbon oxygen content for polycrystalline silicon ingot or purifying furnace according to claim 1, feature exist
In the step（1）The shape that aperture is opened up on middle backplate is unlimited, and the aperture gross area opened up is in 50cm2-150cm2Between,
Aperture position is in mouth of pot between backplate top.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810598214.1A CN108531984A (en) | 2018-06-12 | 2018-06-12 | A method of reducing ingot casting carbon oxygen content for polycrystalline silicon ingot or purifying furnace |
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| CN201810598214.1A CN108531984A (en) | 2018-06-12 | 2018-06-12 | A method of reducing ingot casting carbon oxygen content for polycrystalline silicon ingot or purifying furnace |
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| CN201810598214.1A Pending CN108531984A (en) | 2018-06-12 | 2018-06-12 | A method of reducing ingot casting carbon oxygen content for polycrystalline silicon ingot or purifying furnace |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109321971A (en) * | 2018-12-14 | 2019-02-12 | 扬州荣德新能源科技有限公司 | A kind of abnormal shape polycrystalline furnace crucible guard boards |
| CN112853481A (en) * | 2020-12-31 | 2021-05-28 | 陈富伦 | Preparation method and preparation device of high-purity polycrystalline silicon ingot for cylindrical semiconductor manufacturing process |
-
2018
- 2018-06-12 CN CN201810598214.1A patent/CN108531984A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109321971A (en) * | 2018-12-14 | 2019-02-12 | 扬州荣德新能源科技有限公司 | A kind of abnormal shape polycrystalline furnace crucible guard boards |
| CN112853481A (en) * | 2020-12-31 | 2021-05-28 | 陈富伦 | Preparation method and preparation device of high-purity polycrystalline silicon ingot for cylindrical semiconductor manufacturing process |
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Application publication date: 20180914 |
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| WD01 | Invention patent application deemed withdrawn after publication |