CN109082705A - A kind of quartz crucible coating and its preparation method and application - Google Patents
A kind of quartz crucible coating and its preparation method and application Download PDFInfo
- Publication number
- CN109082705A CN109082705A CN201810818418.1A CN201810818418A CN109082705A CN 109082705 A CN109082705 A CN 109082705A CN 201810818418 A CN201810818418 A CN 201810818418A CN 109082705 A CN109082705 A CN 109082705A
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- CN
- China
- Prior art keywords
- coating
- crucible
- preparation
- sintering aid
- quartz crucible
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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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
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- Chemical & Material Sciences (AREA)
- 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 provides a kind of quartz crucible coatings and its preparation method and application, for the preparation method of the English crucible coating layer the following steps are included: sintering aid in the spray coating liquor of crucible coating layer, is added in (1), mixing is abundant, then it is sprayed on inner surface of crucible, forms coating；(2) after drying to be coated, the inner surface of crucible of coating is heated, dense coating is formed it into.The present invention makes sintering aid form glass phase by adding sintering aid in crucible coating layer spray coating liquor, by pyroprocess, and the bonding beta-silicon nitride powder of these glass forms dense coating in crucible surface in turn.These dense coatings can both play the role of demoulding, be also possible to prevent coating shedding and enter to form Hard Inclusion in silicon crystal, and then stria when reducing multi-wire saw, especially Buddha's warrior attendant wire cutting is bad and broken string risk.
Description
Technical field
The present invention relates to coatings of a kind of silica crucible and preparation method thereof, the life applied to solar power generation silicon crystal
Growth process is particularly suitable for polycrystalline silicon ingot casting process.
Background technique
Solar power generation mainly uses the casting method of directional solidification, in casting process, HIGH-PURITY SILICON with polysilicon at present
Material is placed in silica crucible, melts it completely by heating；Then certain temperature gradient is caused by cooling, keeps silicon molten
Liquid is along certain specific direction directional solidification.In order to smoothly take out the polycrystal silicon ingot being set in silica crucible, avoid silicon liquid solidifying
It causes crucible and silicon ingot to rupture Gu being attached on crucible in the process, needs to coat one layer of release agent in crucible internal walls.It is main at present
The release agent is prepared by the method sprayed using the mixed solution of silicon nitride and water.When high, dry due to spraying liquid water content
Coating shrinkage is big, and silicon nitride fusing point used is high, is difficult to the reasons such as densified sintering product, and release agent coating is in charging and high-temperature fusant stream
It is easy to fall off during dynamic into inside silicon material, there are silicon nitride and the carbonization silas of association in the silicon crystal after leading to solidification
Particle.These impure points silicon wafer cut when, be easy to cause silicon wafer stria it is bad, cutting wire jumper the problems such as, will cause when serious
Cutting broken string.
Summary of the invention
The main object of the present invention is to provide a kind of quartz crucible coating and its preparation method and application, to solve existing skill
Crucible coating layer present in art falls off the problem of leading to Hard Inclusion.
To achieve the above object, the technical solution adopted by the present invention are as follows: a kind of preparation method of quartz crucible coating, including
Following steps: (1) in the spray coating liquor of crucible coating layer, sintering aid is added, mixing sufficiently, is then sprayed at inner surface of crucible
On, form coating；(2) after drying to be coated, the inner surface of crucible of coating is heated, dense coating is formed it into.
In step (1), the sintering aid is one kind of the oxide of silica, aluminium oxide, lithia or rare earth element
Or a variety of mixing, or for the hydroxide or carbonate compound that generate these substances can be decomposed at high temperature.
The form of the sintering aid is powder, it is preferred that the purity of sintering aid is 99%-99.999%, and granularity is
100nm-1mm。
The additive amount of the sintering aid is the 0.5-50wt% of spray coating liquor.
In step (2), the heating method of the inner surface of crucible of coating is electric arc heated or Resistant heating.Heating
Temperature is 600-1700 DEG C, and the time is within 60min.
In step (2), after coating is dry, above-mentioned heating method can not also be used, silicon can be directly loaded into crucible
Material, and put it into and carry out heating and melting and cooling solidification in crystal growing furnace, the heat in crystal growing process is directly utilized,
Crucible coating layer is heated and forms dense coating.
The utility model has the advantages that the present invention makes to be sintered by adding sintering aid in crucible coating layer spray coating liquor by pyroprocess
Auxiliary agent forms glass phase, and the bonding beta-silicon nitride powder of these glass forms dense coating in crucible surface in turn.These densifications apply
Layer can both play the role of demoulding, be also possible to prevent coating shedding and enter to form Hard Inclusion in silicon crystal, and then reduction multi-wire cutting
Cut, especially Buddha's warrior attendant wire cutting when stria it is bad and broken string risk.
Dense coating containing glass phase can also play the metal impurities adsorbed in crucible, the entrance of block carbon oxygen impurities is melted
The effect of body improves the purity and electrical property of crystalline silicon.This is equally applicable monocrystalline silicon growing and its silica crucible used.
Specific embodiment
It is described below for disclosing the present invention so that those skilled in the art can be realized the present invention.It is excellent in being described below
Embodiment is selected to be only used as illustrating, it may occur to persons skilled in the art that other obvious modifications.
Embodiment 1
The sintering aid of spray coating liquor quality 20wt% is added in the spray coating liquor of crucible coating layer in step 1, and mixing is abundant,
Then it is sprayed on inner surface of crucible, forms coating；Wherein, sintering aid is silica, aluminium oxide, lithia or oxidation
One or more mixing of the oxide of the rare earth elements such as yttrium, or for the hydrogen for generating these substances can be decomposed at high temperature
Oxide or carbonate compound, such as aluminium hydroxide, yttrium hydroxide, lithium carbonate.The form of sintering aid is powder, and purity is
99%-99.999%, granularity 100nm-1mm.
Step 2 after drying to be coated, heats the inner surface of crucible of coating, forms it into dense coating.
Heating temperature is being 1200 DEG C, and the time is within 60min；Heating method is electric arc heated.
Step 3 loads silicon material into silica crucible, and puts it into and carry out heating and melting and cooling in crystal growing furnace
Solidification.It after temperature drops to tapping temperature, is drawn off being demoulded, obtains crystalline silicon ingot.
Embodiment 2
The sintering aid of spray coating liquor quality 50wt% is added in the spray coating liquor of crucible coating layer in step 1, and mixing is abundant,
Then it is sprayed on inner surface of crucible, forms coating；Wherein, sintering aid is silica, aluminium oxide, lithia, yttrium oxide
One or more mixing, or for the hydroxide or carbonate compound that generate these substances can be decomposed at high temperature, such as
Aluminium hydroxide, yttrium hydroxide, lithium carbonate etc..The form of sintering aid is powder, and purity 99%-99.999%, granularity is
100nm-1mm。
Step 2 after drying to be coated, heats the inner surface of crucible of coating, forms it into dense coating.
Heating temperature is being 1700 DEG C, and the time is within 60min；Heating method is Resistant heating.
Step 3 loads silicon material into silica crucible, and puts it into and carry out heating and melting and cooling in crystal growing furnace
Solidification.It after temperature drops to tapping temperature, is drawn off being demoulded, obtains crystalline silicon ingot.
Above embodiments are only exemplary embodiment of the present invention, are not used in the limitation present invention, protection scope of the present invention
It is defined by the claims.Those skilled in the art can within the spirit and scope of the present invention make respectively the present invention
Kind modification or equivalent replacement, this modification or equivalent replacement also should be regarded as being within the scope of the present invention.
Claims (7)
1. a kind of preparation method of quartz crucible coating, it is characterised in that: the following steps are included: the spraying of (1) in crucible coating layer
In liquid, sintering aid is added, mixing sufficiently, is then sprayed on inner surface of crucible, forms coating；(2) right after drying to be coated
The inner surface of crucible of coating is heated, and dense coating is formed it into.
2. the preparation method of quartz crucible coating according to claim 1, it is characterised in that: in step (1), the sintering
Auxiliary agent is one or more mixing of the oxide of silica, aluminium oxide, lithia or rare earth element, or in high temperature
The hydroxide or carbonate compound for generating these substances can be decomposed down.
3. the preparation method of quartz crucible coating according to claim 1 or 2, it is characterised in that: the sintering aid
Form is powder, purity 99%-99.999%, granularity 100nm-1mm.
4. the preparation method of quartz crucible coating according to claim 3, it is characterised in that: the addition of the sintering aid
Amount is the 0.5-50wt% of spray coating liquor.
5. the preparation method of quartz crucible coating according to claim 1, it is characterised in that: in step (2), coating
Inner surface of crucible heating method be electric arc heated or Resistant heating.
6. the preparation method of quartz crucible coating according to claim 5, it is characterised in that: heating temperature 600-1700
DEG C, the time is within 60min.
7. the preparation method of quartz crucible coating according to claim 1, it is characterised in that: in step (2), directly to earthenware
Silicon material is loaded in crucible, and puts it into and carries out heating and melting and cooling solidification in crystal growing furnace, directly utilizes crystal growth mistake
Heat in journey, heats crucible coating layer and forms dense coating.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810818418.1A CN109082705A (en) | 2018-07-19 | 2018-07-19 | A kind of quartz crucible coating and its preparation method and application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810818418.1A CN109082705A (en) | 2018-07-19 | 2018-07-19 | A kind of quartz crucible coating and its preparation method and application |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109082705A true CN109082705A (en) | 2018-12-25 |
Family
ID=64838313
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810818418.1A Withdrawn CN109082705A (en) | 2018-07-19 | 2018-07-19 | A kind of quartz crucible coating and its preparation method and application |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109082705A (en) |
-
2018
- 2018-07-19 CN CN201810818418.1A patent/CN109082705A/en not_active Withdrawn
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20181225 |
|
| WW01 | Invention patent application withdrawn after publication |