CN108754601A - A kind of silicon core side ingot manufacturing process of the disconnected ingot of anti-stick pan - Google Patents
A kind of silicon core side ingot manufacturing process of the disconnected ingot of anti-stick pan Download PDFInfo
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- CN108754601A CN108754601A CN201810506441.7A CN201810506441A CN108754601A CN 108754601 A CN108754601 A CN 108754601A CN 201810506441 A CN201810506441 A CN 201810506441A CN 108754601 A CN108754601 A CN 108754601A
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- silicon
- ingot
- crucible
- coating
- core side
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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
-
- 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 present invention relates to a kind of silicon core side ingot manufacturing process of the disconnected ingot of anti-stick pan, the technique includes the following steps：Step 1: crucible spraying is Step 2: dispensing, is then packed into bar shaped crucible by the silicon material prepared；Step 3: needing to carry out vacuumizing operation to furnace body before ingot casting heating; argon gas is continually fed into during heating and is long brilliant in furnace body to be protected; the intake velocity of argon gas is 30L/min during heating melting silicon materials, and the intake velocity of argon gas is 20L/min during long brilliant；Step 4: annealing；Step 5: demoulding of coming out of the stove.A kind of silicon core side ingot manufacturing process of the disconnected ingot of anti-stick pan of the present invention, it coats the first silicon nitride coating at liquid level position after melting silicon materials in crucible by hairbrush, coating compactness is greatly improved compared with thermal spraying mode, melting silicon materials thermal convection current impact can be effective against, prevent coating generation from falling off, to cause silicon ingot to glue the disconnected ingot of crucible.
Description
Technical field
The present invention relates to a kind of silicon core side ingot manufacturing process of the disconnected ingot of anti-stick pan, belong to technical field of polysilicon production.
Background technology
In recent years, increasingly mature with solar energy generation technology, solar cell is all in industry, agricultural and space flight etc.
Multi-field acquirement extensive use.Currently, according to the difference of material therefor, solar cell can be divided into：Silicon solar cell, chemical combination
Object thin-film solar cells and polymer multi-layer modified electrode solar cell, organic solar batteries and nanocrystalline solar electricity
Pond.Wherein, silicon solar cell development is the most ripe, occupies an leading position in the application.Crystal silicon solar energy battery is divided into as list
Crystal silicon solar batteries and polysilicon solar cell.Relative to monocrystaline silicon solar cell, polycrystal silicon cell solar cell
Preparation process is relatively simple, has the advantages that cost low energy is low etc., therefore polysilicon solar cell is using relatively broad.
Crucible is the required equipment of polycrystalline silicon ingot casting production.Currently, production of polysilicon mainly uses silica crucible, this is
Because silica source is abundant, purity is high, and cheap.Although contributed to using silica crucible production polycrystalline silicon ingot casting
Production cost is reduced, but it has a drawback in that silicon ingot easily cracking problem while cooling.This is primarily due to：It is molten
The silicon dioxde reaction that the silicon melted can be in contact with it forms silicon monoxide and oxygen；Wherein, oxygen can pollute silicon, and silicon monoxide has
Volatility；And it can also form silicon carbide and carbon monoxide with the graphite member in stove, and the carbon monoxide of generation then can be with
The pasc reaction of melting, formed volatile silicon monoxide, silicon carbide, the carbide of metallic traces or dopant, oxide and
Carbon, carbon can pollute silicon.Above-mentioned react between silica and molten silicon promotes silicon to be attached on crucible, and due to titanium dioxide
Coefficient of thermal expansion between silicon and silicon both materials is different, and silicon ingot is caused easily to crack while cooling.
Invention content
The technical problem to be solved by the present invention is to provide a kind of silicon core side of the disconnected ingot of anti-stick pan for the above-mentioned prior art
Ingot manufacturing process, it coats the first silicon nitride coating, coating at liquid level position after melting silicon materials in crucible by hairbrush
Compactness is greatly improved compared with thermal spraying mode, can be effective against melting silicon materials thermal convection current impact, prevents coating generation from falling off, from
And silicon ingot is caused to glue the disconnected ingot of crucible.
Technical solution is used by the present invention solves the above problems：A kind of silicon core side ingot manufacture work of the disconnected ingot of anti-stick pan
Skill, the technique include the following steps：
Step 1: crucible spraying
Water and alpha-silicon nitride powders are pressed 1:The first Silicon Nitride, the silicon of theoretical calculation input is made in 1 mass ratio mixing
Liquid level after material fusing in crucible, liquid level position is coated uniformly on using hairbrush by the first Silicon Nitride, is applied
Drying forms the first silicon nitride coating after covering 2~3 times；
Water and alpha-silicon nitride powders are pressed 3.5:1 mass ratio mixing, is made the second Silicon Nitride, using 1.8mm nozzles
It is coated uniformly on crucible internal walls by thermal spraying mode, drying forms the second silicon nitride coating；
Step 2: dispensing, is then packed into bar shaped crucible by the silicon material prepared；
Step 3: ingot casting
The bar shaped crucible for holding silicon material is put into furnace body and is heated, after melting silicon materials, is wanted by the technique of setting
It asks, forms temperature gradient in vertical direction, making the silicon material of fusing, vertically long crystalline form is in strip silicon core in bar shaped crucible
Square ingot；
It needs that furnace body is carried out to vacuumize operation before heating, being continually fed into argon gas in furnace body during heating and is long brilliant carries out
It protects, the intake velocity of argon gas is 30L/min during heating melting silicon materials, and the intake velocity of argon gas is during long brilliant
20L/min；
It anneals Step 4: silicon core side ingot is put into together with bar shaped crucible in sintering furnace；
Step 5: demoulding of coming out of the stove after cooling obtains silicon core side ingot.
Preferably, the thickness of the first silicon nitride coating is 90~100 μm.
Preferably, the width up and down of the first silicon nitride coating is 10cm.
Preferably, the first silicon nitride coating center line is 15cm apart from crucible floor height.
Preferably, the second silicon nitride coating thickness of the first silicon nitride coating position coating is 90~100 μm, remaining position
The thickness of second silicon nitride coating is 180~200 μm.
Compared with the prior art, the advantages of the present invention are as follows：
1, the present invention coats the first silicon nitride coating at liquid level position after melting silicon materials in crucible by hairbrush, applies
Layer compactness is greatly improved compared with thermal spraying mode, can be effective against melting silicon materials thermal convection current impact, prevents coating generation from falling off,
To cause silicon ingot to glue the disconnected ingot of crucible；
2, the present invention is protected during heating and long crystalline substance by being continually fed into argon gas, and the design conjunction of argon inlet amount
Reason can prevent from generating impact to silicon liquid, effectively inhibit silicon liquid to nitrogen in crucible in the case where ensureing end product quality
SiClx coating washes away, and the quality of final silicon core side ingot has been effectively ensured.
Description of the drawings
Fig. 1 is the structural schematic diagram after crucible spraying in a kind of silicon core side ingot manufacturing process of the disconnected ingot of anti-stick pan of the present invention.
Wherein：
Crucible body 1
Bottom plate 11
Side plate 12
Storage cavity 2
First silicon nitride coating 3
Second silicon nitride coating 4.
Specific implementation mode
Below in conjunction with attached drawing embodiment, present invention is further described in detail.
A kind of silicon core side ingot manufacturing process of the disconnected ingot of anti-stick pan in the present embodiment, the technique include the following steps：
Step 1: crucible spraying
Water and alpha-silicon nitride powders are pressed 1:The first Silicon Nitride, the silicon of theoretical calculation input is made in 1 mass ratio mixing
Liquid level after material fusing in crucible, liquid level position is coated uniformly on using hairbrush by the first Silicon Nitride, is applied
Drying forms the first silicon nitride coating after covering 2~3 times；
The thickness of first silicon nitride coating is 90~100 μm；The width up and down of first silicon nitride coating is 10cm, the first nitrogen
SiClx coated center linear distance crucible floor height is 15cm；
Water and alpha-silicon nitride powders are pressed 3.5:1 mass ratio mixing, is made the second Silicon Nitride, using 1.8mm nozzles
It is coated uniformly on crucible internal walls by thermal spraying mode and (may include the first silicon nitride coating position), drying forms the second nitridation
It is as shown in Figure 1 to coat the crucible formed after the completion for silicon coating；
Second silicon nitride coating thickness of the first silicon nitride coating position coating is 90~100 μm, remaining second nitrogen of position
The thickness of SiClx coating is 180~200 μm；
Step 2: dispensing, is then packed into bar shaped crucible by the silicon material prepared；
Step 3: ingot casting
The bar shaped crucible for holding silicon material is put into furnace body and is heated, after melting silicon materials, is wanted by the technique of setting
It asks, forms temperature gradient in vertical direction, making the silicon material of fusing, vertically long crystalline form is in strip silicon core in bar shaped crucible
Square ingot；
It needs that furnace body is carried out to vacuumize operation before heating, being continually fed into argon gas in furnace body during heating and is long brilliant carries out
It protects, the intake velocity of argon gas is 30L/min during heating melting silicon materials, and the intake velocity of argon gas is during long brilliant
20L/min；
It anneals Step 4: silicon core side ingot is put into together with bar shaped crucible in sintering furnace；
Step 5: demoulding of coming out of the stove after cooling obtains silicon core side ingot.
In addition to the implementation, all to use equivalent transformation or equivalent replacement the invention also includes there is an other embodiment
The technical solution that mode is formed should all be fallen within the scope of the hereto appended claims.
Claims (5)
- The silicon core side ingot manufacturing process of ingot 1. a kind of anti-stick pan is broken, it is characterised in that the technique includes the following steps：Step 1: crucible sprayingWater and alpha-silicon nitride powders are pressed 1:1 mass ratio mixing, is made the first Silicon Nitride, and the silicon material of theoretical calculation input is molten First Silicon Nitride is coated uniformly on liquid level position by the liquid level after change in crucible using hairbrush, and coating 2~ Drying forms the first silicon nitride coating after 3 times；Water and alpha-silicon nitride powders are pressed 3.5:1 mass ratio mixing, is made the second Silicon Nitride, is passed through using 1.8mm nozzles Thermal spraying mode is coated uniformly on crucible internal walls, and drying forms the second silicon nitride coating；Step 2: dispensing, is then packed into bar shaped crucible by the silicon material prepared；Step 3: ingot castingThe bar shaped crucible for holding silicon material is put into furnace body and is heated, after melting silicon materials, presses the technological requirement of setting, Vertical direction forms temperature gradient, and making the silicon material of fusing, vertically long crystalline form is in strip silicon core side ingot in bar shaped crucible；It needs that furnace body is carried out to vacuumize operation before heating, being continually fed into argon gas in furnace body during heating and is long brilliant is protected It protects, the intake velocity of argon gas is 30L/min during heating melting silicon materials, and the intake velocity of argon gas is 20L/ during long brilliant min；It anneals Step 4: silicon core side ingot is put into together with bar shaped crucible in sintering furnace；Step 5: demoulding of coming out of the stove after cooling obtains silicon core side ingot.
- The silicon core side ingot manufacturing process of ingot 2. a kind of anti-stick pan according to claim 1 is broken, it is characterised in that：First nitridation The thickness of silicon coating is 90~100 μm.
- The silicon core side ingot manufacturing process of ingot 3. a kind of anti-stick pan according to claim 1 is broken, it is characterised in that：First nitridation The width up and down of silicon coating is 10cm.
- The silicon core side ingot manufacturing process of ingot 4. a kind of anti-stick pan according to claim 1 is broken, it is characterised in that：First nitridation Silicon coating center line is 15cm apart from crucible floor height.
- The silicon core side ingot manufacturing process of ingot 5. a kind of anti-stick pan according to claim 1 is broken, it is characterised in that：First nitridation Second silicon nitride coating thickness of silicon coating position coating is 90~100 μm, and the thickness of remaining the second silicon nitride coating of position is 180~200 μm.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810506441.7A CN108754601A (en) | 2018-05-24 | 2018-05-24 | A kind of silicon core side ingot manufacturing process of the disconnected ingot of anti-stick pan |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810506441.7A CN108754601A (en) | 2018-05-24 | 2018-05-24 | A kind of silicon core side ingot manufacturing process of the disconnected ingot of anti-stick pan |
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| CN108754601A true CN108754601A (en) | 2018-11-06 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102909163A (en) * | 2011-08-05 | 2013-02-06 | 镇江仁德新能源科技有限公司 | Method for forming coating on inner surface of polycrystalline silicon ingot casting crucible |
| CN203513830U (en) * | 2013-08-13 | 2014-04-02 | 常熟华融太阳能新型材料有限公司 | Quartz ceramic crucible capable of reducing content of oxygen and carbon for polycrystalline silicon ingot |
| CN104109902A (en) * | 2014-05-16 | 2014-10-22 | 江西赛维Ldk太阳能高科技有限公司 | Crucible for polysilicon ingot casting, coating structure of crucible and coating preparation method |
| CN204385319U (en) * | 2014-12-31 | 2015-06-10 | 惠梦君 | A kind of horizontal zone melting polycrystalline silicon ingot or purifying furnace |
| CN107417301A (en) * | 2017-08-18 | 2017-12-01 | 晶科能源有限公司 | A kind of silicon nitride coating preparation method of quartz crucible for casting polycrystalline silicon ingot |
| CN107747124A (en) * | 2017-11-07 | 2018-03-02 | 晶科能源有限公司 | A kind of anti-sticking crucible method of polycrystalline cast ingot |
-
2018
- 2018-05-24 CN CN201810506441.7A patent/CN108754601A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102909163A (en) * | 2011-08-05 | 2013-02-06 | 镇江仁德新能源科技有限公司 | Method for forming coating on inner surface of polycrystalline silicon ingot casting crucible |
| CN203513830U (en) * | 2013-08-13 | 2014-04-02 | 常熟华融太阳能新型材料有限公司 | Quartz ceramic crucible capable of reducing content of oxygen and carbon for polycrystalline silicon ingot |
| CN104109902A (en) * | 2014-05-16 | 2014-10-22 | 江西赛维Ldk太阳能高科技有限公司 | Crucible for polysilicon ingot casting, coating structure of crucible and coating preparation method |
| CN204385319U (en) * | 2014-12-31 | 2015-06-10 | 惠梦君 | A kind of horizontal zone melting polycrystalline silicon ingot or purifying furnace |
| CN107417301A (en) * | 2017-08-18 | 2017-12-01 | 晶科能源有限公司 | A kind of silicon nitride coating preparation method of quartz crucible for casting polycrystalline silicon ingot |
| CN107747124A (en) * | 2017-11-07 | 2018-03-02 | 晶科能源有限公司 | A kind of anti-sticking crucible method of polycrystalline cast ingot |
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Application publication date: 20181106 |