CN110016715A - A kind of preparation method of polycrystalline cast ingot crucible coating layer - Google Patents
A kind of preparation method of polycrystalline cast ingot crucible coating layer Download PDFInfo
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- CN110016715A CN110016715A CN201910192533.7A CN201910192533A CN110016715A CN 110016715 A CN110016715 A CN 110016715A CN 201910192533 A CN201910192533 A CN 201910192533A CN 110016715 A CN110016715 A CN 110016715A
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- crucible
- cast ingot
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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
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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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- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The present invention relates to a kind of preparation methods of polycrystalline cast ingot crucible coating layer, include the following steps: for thermostable heat-isolating coating to be coated uniformly on crucible body low-temperature region lateral wall, there is crucible surface after brushing without obvious visual exposed quartz, the baking of independent closed spacing high-temperature is solidificated in it on crucible lateral wall, takes out after cooling；The thermostable heat-isolating coating is made of nano ceramics microballon, silicate compound and water, and the low-temperature region refers to the part that crystal grain is grown in the diagonal in crucible.The excellent adsorption of polycrystalline cast ingot crucible coating layer and crucible surface that the present invention obtains, adhesion strength is high, is not subject to destroy, uniformity of temperature profile, advantageously forms the long crystal boundary face of intermediate dimpling, improve the transfer efficiency of polysilicon chip.
Description
Technical field
The present invention relates to a kind of polycrystalline cast ingot sintering process, in particular to a kind of polycrystalline cast ingot crucible coating layer
Preparation method.
Background technique
Manufacture polysilicon chip needs to use a kind of important equipment-crucible, the technical solution generallyd use in industry at present
For the intracavitary temperature unification of ingot furnace is reduced by way of technique adjustment in inner surface of crucible, make the outer of areas of higher temperature
Inclined crystal grain straightens, and reduces since the intracavitary temperature of ingot furnace is unified, the former lower regional temperature of temperature is lower, in crystal grain tiltedly more
Seriously, for such situation, one layer of silicon nitride coating is made as release agent, so that it is guaranteed that in the ingot casting stage in inner surface of crucible
Silicon liquid does not occur directly to contact with crucible, reduces the risk that viscous pot splits ingot, although this technical solution comparative maturity at present,
The asymmetry of polycrystalline ingot furnace electrode causes ingot casting furnace chamber temperature to be unevenly distributed, some regional temperatures are relatively low, brilliant
Grain sideling ingrowing；Some regional temperatures are relatively high, and crystal grain is sideling to outgrowth.When crystal grain is grown along vertical direction
When, crystal defect is less, and defect value-added speed is slower, and cell piece efficiency is higher；Crystal grain sideling grows that will lead to crystal defect fast
Speed increment, to reduce the efficiency of cell piece.
Summary of the invention
The purpose of the present invention is to overcome the deficiency in the prior art, provides a kind of preparation side of polycrystalline cast ingot crucible coating layer
Method, the excellent adsorption of polycrystalline cast ingot crucible coating layer and crucible surface that the present invention obtains, adhesion strength is higher, is not subject to brokenly
Bad, uniformity of temperature profile advantageously forms the long crystal boundary face of intermediate dimpling, improves the transfer efficiency of polysilicon chip.
The technical solution adopted by the present invention to solve the technical problems is:
A kind of preparation method of polycrystalline cast ingot crucible coating layer, includes the following steps: uniformly to apply thermostable heat-isolating coating
Crucible body low-temperature region lateral wall is overlayed on, has crucible surface after brushing without obvious visual exposed quartz, independent closed
Spacing high-temperature baking is solidificated in it on crucible lateral wall, takes out after cooling；The thermostable heat-isolating coating is made pottery by nanometer
Porcelain microballon, silicate compound and water composition, the low-temperature region is the region that crystal grain is grown in the diagonal in crucible.
The crucible body is by quartz material or silicon nitride material casting and forming as a preferred technical solution,.
The crucible body is square tube shape as a preferred technical solution,.
The mass ratio of the nano ceramics microballon, silicate compound and water is 1~10 as a preferred technical solution:
20~45:45~65.
The silicate compound dosage is 100-1000g/ crucible as a preferred technical solution,.
The silicate compound includes alumina silicate, ferrosilite, calcium silicates, magnesium silicate, silicon as a preferred technical solution,
One of sour potassium, sodium metasilicate are a variety of.
The position of the heat insulation coating, height, width, thickness can be according to close to crucibles as a preferred technical solution,
The crystal grain of edge crystal bar intilted size is adjusted, with the raising of inclined degree, the thickness of heat insulation coating also phase
It should improve.
The thickness of the heat insulation coating is between 1-30mm as a preferred technical solution,.
The temperature of the drying is 30~60 DEG C as a preferred technical solution, preferably 30 DEG C, 40 DEG C, 60 DEG C；It is described
Drying time is 1~12h, preferably 1h, 6h, 12h.
The coating coating method is brushing, roller coating or spraying as a preferred technical solution, and coating number is 1-40
It is secondary.
By above technical scheme, compared with the existing technology, the invention has the following advantages:
1, thermal insulation coatings fire-protection rating of the invention is A grades, non-ignitable, can prevent the generation of dew condensation phenomenon, is free of harmful substance VOC
Ingredients are waited, will not be caused harm to the human body in construction and use process；
2. being in low-temperature region part brush heat insulation coating in crucible, the plagioclase crystalline substance that can significantly eliminate crucible inside edge crystal is existing
As reducing dislocation density, reducing scattering and disappearing for crystal growing stage heat, promote crystal grain to grow along the vertical direction, improve polysilicon chip
Or the transfer efficiency of class monocrystalline silicon piece；
3. operation of the present invention step is simple, it is only necessary to according to crucible different location profiling temperatures, paint respective area and thickness
The thermal insulation coatings of degree, play function of heat insulation；
4. the present invention is applied widely, more than for producing polysilicon chip, it may also be used for production monocrystalline silicon piece.
Detailed description of the invention
Present invention will be further explained below with reference to the attached drawings and examples:
Fig. 1 is the main view of polycrystalline cast ingot crucible of the present invention；
In figure: 1- crucible body, 2- thick coating, 3- shallow layer, 4- bottom plate.
Specific embodiment
In conjunction with the accompanying drawings, the present invention is further explained in detail.These attached drawings are simplified schematic diagram, only with
Illustration illustrates basic structure of the invention, therefore it only shows the composition relevant to the invention.
The present invention has no special limitation to the coating equipment, is using coating equipment well known to those skilled in the art
It can.In an embodiment of the present invention, described applied to spraying, roller coating or brushing.
Low-temperature region of the present invention refers to the part that crystal grain is grown in the diagonal in crucible.
The present invention has no special limitation to the method for the stirring, using stirring means well known to those skilled in the art
?.
The shape of crucible body 1 of the invention can there are many, the shape of the silicon ingot depending on required casting, such as Fig. 1
Shown, crucible body 1 can be square tube shape.
Brushing mode used in the embodiment of the present invention uses common hairbrush, and hair loss person is not advisable, and round brush selects common round brush,
Hair loss person is not advisable.
The position of heat insulation coating of the present invention, height, width, thickness can be according to the crystalline substances close to crucible edge crystal bar
Grain intilted size is adjusted, and with the raising of inclined degree, the thickness of heat insulation coating is also improved.
In order to further illustrate the present invention, a kind of polycrystalline cast ingot provided by the invention is applied with crucible with reference to embodiments
The preparation method and crucible of layer are described in detail, but cannot be understood as limiting the scope of the present invention.Following reality
The source for applying raw material components used in example has no special limitation, can be general commercially available.
Embodiment 1
Nano ceramics microballon, silicate compound and the water that 500g mass ratio is 1:20:65 are weighed, is uniformly mixed, obtains
Silicate mixed slurry；
Mixed slurry is coated uniformly on the low-temperature region lateral wall of crucible body by brushing or roller applications, makes earthenware after coating
Crucible surface exists without obvious visual exposed quartz.According to crystal grain in crucible, extent of growth determines coating number in the diagonal, inclines
It is tiltedly more obvious, in order to achieve the effect that heat preservation coating number is more.Specific method is using multilayer construction method, the thickness of first layer
In 0.3mm or so, every layer of thickness control is in 0.5mm~0.8mm later.When multilayer is constructed, after the preceding layers dry tack free such as need
Can construct next layer, and later layer brushing direction is vertical with preceding layer direction, at room temperature the coating surface dry time
About 1 hour, surface temperature was higher, and the waiting time is shorter, and the present embodiment drying temperature is 60 DEG C, brushes or roller coating number is
40 times, coating layer thickness is between 1-30mm, when being brushed using brush, roller, needs to be overlapped 10cm when being connected between per pass, prevent
Holiday；
It is cooled to room temperature after drying, obtains the polycrystalline cast ingot crucible that bottom section lateral wall has heat insulation coating；
For the crucible body of the present embodiment by quartz material casting and forming, crucible body is square tube shape, and silicate compound can be
Alumina silicate, the position of heat insulation coating, height, width, brushing thickness can be lean-in according to the crystal grain close to crucible edge crystal bar
Oblique size is adjusted, and with the raising of inclined degree, the thickness of heat insulation coating also correspondinglys increase.
Embodiment 2
The present embodiment difference from example 1 is that, crucible body is by silicon nitride material casting and forming.The nano ceramics
The mass ratio of microballon, silicate compound and water is 5:35:45, and silicate compound dosage is 100g/ crucible, silicate compounds
Object is that ferrosilite drying temperature is 40 DEG C, drying time 6h, and coating coating method is roller coating, and coating number is 25 times.
Embodiment 3
The present embodiment difference from example 1 is that, crucible body is by silicon nitride material casting and forming.The nano ceramics
The mass ratio of microballon, silicate compound and water is 1:45:60, and heat insulation coating dosage is 800g/ crucible, and silicate compound is
Calcium silicates, drying temperature are 50 DEG C, drying time 3h, and coating coating method is spraying, and coating number is 30 times.
Embodiment 4
The present embodiment difference from example 1 is that, crucible body is by quartz material casting and forming.The nano ceramics is micro-
The mass ratio of pearl, silicate compound and water is 5:35:60, and heat insulation coating dosage is 1000g/ crucible, and silicate compound is
Potassium silicate, the temperature of the drying are 30 DEG C；Drying time is 12h, and coating coating method is to brush, and coating number is 20 times.
Table 1 is using the silicon wafer efficiency after the energy saving polycrystalline ingot furnace of embodiment 1 and embodiment 2 with common polycrystalline ingot furnace
The data comparison of (silicon wafer of energy saving polycrystalline ingot furnace production through the invention converts light energy into the efficiency of electric energy):
Table 1: common polycrystalline ingot furnace and the present embodiment polycrystalline ingot furnace data comparison
| The type of ingot furnace | Silicon wafer transfer efficiency % |
| Common polycrystalline ingot furnace | 18.85 |
| 1 polycrystalline ingot furnace of embodiment | 18.90 |
| 2 polycrystalline ingot furnace of embodiment | 18.88 |
| 3 polycrystalline ingot furnace of embodiment | 18.89 |
| 4 polycrystalline ingot furnace of embodiment | 18.91 |
By above data as it can be seen that the polycrystalline cast ingot silicon wafer high conversion efficiency of applying coating of the present invention, it is clear that be because use is led
The hot lower thermostable heat-isolating coating of coefficient reduces scattering and disappearing for low-temperature region crystal growing stage heat, makes furnace chamber temperature
It is distributed more uniform, crystal grain is grown along the vertical direction, is formed the long crystal boundary face of one dimpling of formation of a dimpling, is produced
The silicon wafer of better quality.
Taking the above-mentioned ideal embodiment according to the present invention as inspiration, through the above description, relevant staff is complete
Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.The technology of this invention
Property range is not limited to the contents of the specification, it is necessary to which the technical scope thereof is determined according to the scope of the claim.
Claims (10)
1. a kind of preparation method of polycrystalline cast ingot crucible coating layer, which comprises the steps of: protect high temperature resistant heat insulation
Thermo-paint is coated uniformly on crucible body low-temperature region lateral wall, deposits crucible surface after brushing without obvious visual exposed quartz
It is solidificated on crucible lateral wall in the baking of, independent closed spacing high-temperature, is taken out after cooling；The thermostable heat-isolating applies
Material is made of nano ceramics microballon, silicate compound and water, and the low-temperature region is the area that crystal grain is grown in the diagonal in crucible
Domain.
2. the preparation method of polycrystalline cast ingot crucible coating layer as described in claim 1, which is characterized in that the crucible body by
Quartz material or silicon nitride material casting and forming.
3. the preparation method of polycrystalline cast ingot crucible coating layer as described in claim 1, which is characterized in that the crucible body is
Square tube shape.
4. the preparation method of polycrystalline cast ingot crucible coating layer as described in claim 1, which is characterized in that the nano ceramics is micro-
The mass ratio of pearl, silicate compound and water is 1~10:20~45:45~65.
5. the preparation method of polycrystalline cast ingot crucible coating layer as described in claim 1, which is characterized in that the silicate compounds
Object dosage is 100-1000g/ crucible.
6. the preparation method of polycrystalline cast ingot crucible coating layer as described in claim 1, which is characterized in that the silicate compounds
Object includes one of alumina silicate, ferrosilite, calcium silicates, magnesium silicate, potassium silicate, sodium metasilicate or a variety of.
7. the preparation method of polycrystalline cast ingot crucible coating layer as described in claim 1, which is characterized in that the heat insulation coating
Position, height, width, thickness can be adjusted according to the intilted size of crystal grain close to crucible edge crystal bar.
8. the preparation method of polycrystalline cast ingot crucible coating layer as claimed in claim 7, which is characterized in that the heat insulation coating
Thickness is between 1-30mm.
9. the preparation method of polycrystalline cast ingot crucible coating layer as described in claim 1, which is characterized in that the temperature of the drying
It is 30~60 DEG C, preferably 30 DEG C, 40 DEG C, 60 DEG C；The drying time is 1~12h, preferably 1h, 6h, 12h.
10. the preparation method of polycrystalline cast ingot crucible coating layer as described in claim 1, which is characterized in that the coating coating
Mode is brushing, roller coating or spraying, and coating number is 1-40 times.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910192533.7A CN110016715A (en) | 2019-03-14 | 2019-03-14 | A kind of preparation method of polycrystalline cast ingot crucible coating layer |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910192533.7A CN110016715A (en) | 2019-03-14 | 2019-03-14 | A kind of preparation method of polycrystalline cast ingot crucible coating layer |
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| CN110016715A true CN110016715A (en) | 2019-07-16 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1058091A (en) * | 1990-06-06 | 1992-01-22 | 联合碳化涂料服务技术公司 | Borium nitride crucible and manufacture method thereof |
| JP2005029405A (en) * | 2003-07-09 | 2005-02-03 | Sharp Corp | Plate-like silicon manufacturing apparatus |
| CN105803525A (en) * | 2016-04-05 | 2016-07-27 | 晶科能源有限公司 | Crucible and crucible manufacturing method |
| CN107759189A (en) * | 2016-08-22 | 2018-03-06 | 银川隆基硅材料有限公司 | Thermostable heat-isolating coating and the method for improving single crystal growing furnace crucible side service life |
-
2019
- 2019-03-14 CN CN201910192533.7A patent/CN110016715A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1058091A (en) * | 1990-06-06 | 1992-01-22 | 联合碳化涂料服务技术公司 | Borium nitride crucible and manufacture method thereof |
| JP2005029405A (en) * | 2003-07-09 | 2005-02-03 | Sharp Corp | Plate-like silicon manufacturing apparatus |
| CN105803525A (en) * | 2016-04-05 | 2016-07-27 | 晶科能源有限公司 | Crucible and crucible manufacturing method |
| CN107759189A (en) * | 2016-08-22 | 2018-03-06 | 银川隆基硅材料有限公司 | Thermostable heat-isolating coating and the method for improving single crystal growing furnace crucible side service life |
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