CN109267150A - A kind of composite construction quartz ceramic crucible and preparation method thereof - Google Patents
A kind of composite construction quartz ceramic crucible and preparation method thereof Download PDFInfo
- Publication number
- CN109267150A CN109267150A CN201811158982.1A CN201811158982A CN109267150A CN 109267150 A CN109267150 A CN 109267150A CN 201811158982 A CN201811158982 A CN 201811158982A CN 109267150 A CN109267150 A CN 109267150A
- Authority
- CN
- China
- Prior art keywords
- crucible
- glass sand
- composite construction
- partial size
- quartz
- 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.)
- Pending
Links
Classifications
-
- 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
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Metallurgy (AREA)
- Structural Engineering (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The present invention provides a kind of composite construction quartz ceramic crucibles, the composite construction quartz ceramic crucible include crucible body and be arranged in the crucible body all or part of inner surface high purity quartz layer, the material of the high purity quartz layer includes the glass sand that purity is greater than 99.99% and partial size is no more than 5mm, wherein, granular mass accounting of the partial size greater than 2mm is 10%-35% in the glass sand.When the composite construction quartz ceramic crucible carries out polycrystalline silicon ingot casting, it is possible to reduce impurity content and oxygen content in silicon ingot reduce the red side phenomenon of silicon ingot, obtain the polycrystal silicon ingot of high quality.
Description
Technical field
The present invention relates to quartz ceramic crucible technical field, in particular to a kind of composite construction quartz ceramic crucible and its system
Preparation Method.
Background technique
Quartz ceramic crucible is that polycrystalline silicon ingot casting process loads polycrystalline silicon raw material, by heating, fusing, long crystalline substance, is annealed, cold
But the stage obtains the container of polycrystal silicon ingot.Quartz ceramic crucible is generally made of purity of 99.9% quartz sand, although quartzy
Ceramic crucible inner wall has silicon nitride coating isolation, but still has a large amount of dopants penetrations into silicon ingot in ingot casting, especially ferro element,
Copper etc..The above problem can be effectively improved using body high purity quartz ceramic crucible prepared by glass sand, but it is high-purity
The cost of quartz sand is 10 times of common quartz sand or so, and production cost is too high unbearable.Quartz ceramic crucible is burnt at present
After knot, high purity quartz slurry is prepared one in quartz ceramic crucible inner wall by the methods of brushing, spraying, roller coating, curtain coating, dipping
Layer high purity quartz barrier layer, obstructs the diffusion of impurity in crucible.But the high purity quartz barrier layer compactness is not high, reactivity
It is high, poor with the adhesion of silicon nitride coating, cause silicon ingot to still have the red side of 5mm-10mm, while the oxygen content in silicon ingot increases
Add 2ppm-4ppm, the shortcomings that there are silicon nitride lodging, silicon nitride inclusions, Hard Inclusion in silicon ingot dramatically increase, so that silicon ingot goes out
Material rate reduces, and increases the initial photo attenuation in battery component, transfer efficiency is remarkably decreased, the cutting in Buddha's warrior attendant wire cutting
Yield rate is remarkably decreased.Therefore, being badly in need of one kind can be to avoid the quartz ceramic crucible of prior art defect.
Summary of the invention
In view of this, the present invention provides a kind of composite construction quartz ceramic crucible, including crucible body and setting exist
The high purity quartz layer of all or part of inner surface of the crucible body, the material of the high purity quartz layer include that purity is greater than
99.99% and partial size be no more than 5mm glass sand, wherein in the glass sand partial size be greater than 2mm granular mass
Accounting is 10%-35%.When the composite construction quartz ceramic crucible carries out polycrystalline silicon ingot casting, it is possible to reduce impurity content in silicon ingot
And oxygen content, the red side phenomenon of silicon ingot is reduced, the polycrystal silicon ingot of high quality is obtained.
In a first aspect, the present invention provides a kind of composite construction quartz ceramic crucible, the composite construction quartz-ceramics earthenware
Crucible include crucible body and be arranged in the crucible body all or part of inner surface high purity quartz layer, high-purity stone
The material of English layer includes the glass sand that purity is greater than 99.99% and partial size is no more than 5mm, wherein the glass sand
Granular mass accounting of the middle partial size greater than 2mm is 10%-35%.
In the present invention, the partial size and composition ratio for controlling glass sand high purity quartz layer can be made more uniform with
And stablize, to be conducive to the production of polycrystal silicon ingot.
Optionally, in the high purity quartz layer, the glass sand passes through the three of the monomer crosslinked formation of organic polymer
Dimension reticular structure is bound up.
Optionally, the mass content of glass sand described in the high purity quartz layer is greater than 97%.Further, described
The mass content of glass sand described in high purity quartz layer is greater than 98%, 99% or 99.3%
In the present invention, glass sand is bound up on one by the tridimensional network of the monomer crosslinked formation of organic polymer
It rises, is evenly distributed in the tridimensional network of the monomer crosslinked formation of organic polymer to be conducive to glass sand, with
So that high purity quartz layer is preferably adhered in crucible body.
Optionally, the organic polymer monomer is the compound containing multiple functional groups.It is further alternative, it is described to have
Machine polymer monomer includes at least one of acrylamide, Methacrylamide and hydroxymethyl acrylamide.
Optionally, the glass sand includes coarse aggregate glass sand and fine powder material glass sand, described high-purity
The mass ratio of coarse aggregate glass sand described in quartz layer and the fine powder material glass sand is 1:(1-4), the thick bone
The partial size for expecting glass sand is 0.5mm-5mm, and the partial size of the fine powder material glass sand is less than 0.5mm.
Optionally, the fine powder material glass sand is made of by quality accounting following different-grain diameter particle:
Partial size is greater than 0.1mm and is less than 0.5mm 10%-30%
Partial size 0.05mm-0.1mm 30%-60%
Partial size is less than 0.05mm 30%-60%.
Optionally, the coarse aggregate glass sand is made of by quality accounting following different-grain diameter particle:
Partial size is greater than 2mm and is no more than 5mm 50%-70%
Partial size 1mm-2mm 20%-40%
Partial size is not less than 0.5mm and is less than 1mm 10%-30%.
Optionally, the bulk density of the composite construction quartz ceramic crucible is greater than 1.9g/cm3.It is further alternative, institute
The bulk density for stating composite construction quartz ceramic crucible is greater than 1.94g/cm3。
Optionally, the roughness of the high purity quartz layer is 5 μm -50 μm.
Optionally, the high purity quartz layer with a thickness of 0.1mm-20mm.Further, the thickness of the high purity quartz layer
For 1mm-15mm.
Optionally, the high purity quartz layer is equal thickness, progressive thickness or graded thickness.
Optionally, the high purity quartz layer increases in the thickness of the estimated stops of silicon liquid level of solution, and the crucible body
Reduce in the thickness of the estimated stops of the silicon liquid level of solution, the thickness of the composite construction quartz ceramic crucible remains unchanged.
Optionally, the surface of the high purity quartz layer is coated with silicon nitride layer.
Optionally, the composite construction quartz ceramic crucible with a thickness of 20mm-30mm.
First aspect present invention provides a kind of composite construction quartz ceramic crucible, and inner surface has high purity quartz layer,
The material of the high purity quartz layer includes that purity is greater than 99.99% and glass sand of the partial size no more than 5mm, and high purity quartz
Granular mass accounting of the partial size greater than 2mm is 10%-35% in sand.The present invention in crucible body by being arranged high purity quartz
Layer, the purity of silicon wafer when improving subsequent polycrystalline silicon ingot casting, meanwhile, it include the biggish particle of partial size in the high purity quartz layer,
It will not be displaced when being formed by curing high purity quartz layer, to improve the stability of high purity quartz layer, be conducive to high purity quartz layer
With being bonded for crucible body, the binding force of high purity quartz layer and crucible body is improved.The composite construction stone prepared through the invention
When English ceramic crucible carries out polycrystalline silicon ingot casting, it is possible to reduce impurity content and oxygen content in silicon ingot reduce the red side phenomenon of silicon ingot,
Obtain the polycrystal silicon ingot of high quality.
Second aspect, the present invention provides a kind of preparation methods of composite construction quartz ceramic crucible, comprising:
By glass sand and water mixed grinding at quartz slurry, the purity of the glass sand be greater than 99.99% and
Partial size is no more than 5mm, wherein granular mass accounting of the partial size greater than 2mm is 10%-35% in the glass sand；To institute
It states and organic polymer monomer, crosslinking agent and initiator is added in quartz slurry, be uniformly mixed and form mixed slurry；
Crucible body is taken, the mixed slurry is injected by the crucible body using gel-casting, it is cured to make the earthenware
High purity quartz layer is formed on all or part of inner surface of crucible ontology, roughened processing obtains composite construction quartz-ceramics earthenware
Crucible.
In the present invention, using the glass sand of certain pure and partial size, and organic polymer monomer, crosslinking agent is added
Mixed slurry, which is formed, with initiator forms high purity quartz on all or part of inner surface of crucible body using gel-casting
Layer prevents impurity diffusion during polycrystalline silicon ingot casting in crucible body into silicon ingot, reduces production cost；Meanwhile it using
Gel-casting can be such that high purity quartz layer is preferably attached in crucible body, and can also use the high purity quartz of bulky grain
Sand is conducive to the stability of composite construction quartz ceramic crucible entirety.
It is in the prior art using the methods of brushing, spraying, roller coating, curtain coating, dipping in crucible body inner surface system
Standby one layer of high purity quartz layer, but its compactness is not high, reactivity is high, poor with the adhesion of silicon nitride coating, and the present invention adopts
With the solidifying mode of note, solidification obtains high purity quartz layer, and through oversintering, compactness is improved, and reactivity significantly reduces, Ke Yiyou
Effect reduces the oxygen content in silicon ingot, is easy to adhere to silicon nitride layer, reduces the content of silicon nitride in silicon ingot；Secondly, use brushing,
The methods of spraying, roller coating, curtain coating, dipping are required to the glass sand using partial size smaller (such as partial size is no more than 2mm), and originally
The biggish glass sand of partial size can be used in invention, and the different glass sand of partial size can uniformly divide in mixed slurry
Cloth, and be not displaced in the curing process, improve the stability of crucible.
Optionally, the glass sand includes coarse aggregate glass sand and fine powder material glass sand, described high-purity
The mass ratio of coarse aggregate glass sand described in quartz layer and the fine powder material glass sand is 1:(1-4), the thick bone
The partial size for expecting glass sand is 0.5mm-5mm, and the partial size of the fine powder material glass sand is less than 0.5mm.
Optionally, the fine powder material glass sand is made of by quality accounting following different-grain diameter particle:
Partial size is greater than 0.1mm and is less than 0.5mm 10%-30%
Partial size 0.05mm-0.1mm 30%-60%
Partial size is less than 0.05mm 30%-60%.
Optionally, the coarse aggregate glass sand is made of by quality accounting following different-grain diameter particle:
Partial size is greater than 2mm and is no more than 5mm 50%-70%
Partial size 1mm-2mm 20%-40%
Partial size is not less than 0.5mm and is less than 1mm 10%-30%.
Optionally, in the high purity quartz layer, the glass sand passes through the three of the monomer crosslinked formation of organic polymer
Dimension reticular structure is bound up.
Optionally, the solid concentration of the quartz slurry is greater than 90%wt.
Optionally, it is described by glass sand and water mixed grinding at quartz slurry, comprising:
Using a step polishing or multistep polishing, the glass sand is mixed with water, and abrasive media is added and exists
It is ground in milling apparatus, the quartz slurry is made.
Further, the abrasive media includes in zirconia ball, silicon nitride ball, agate ball, alumina balls and corundum ball
At least one.Further, the milling apparatus include in planetary ball mill, horizontal ball mill and vertical ball mill extremely
Few one kind.
Optionally, the organic polymer monomer is the compound containing multiple functional groups.It is further alternative, it is described to have
Machine polymer monomer includes at least one of acrylamide, Methacrylamide and hydroxymethyl acrylamide.
Optionally, the quality accounting of organic polymer monomer described in the mixed slurry is 0.1%-5%.
Optionally, the crosslinking agent is the compound containing multiple functional groups.Further alternative, the crosslinking agent includes
At least one of middle N,N methylene bis acrylamide, divinylbenzene and diisocyanate.
Optionally, the quality accounting of crosslinking agent described in the mixed slurry is the organic polymer monomer mass
0.1%-5%.
Optionally, the initiator includes at least one of ammonium persulfate, azodiisobutyronitrile and azobisisoheptonitrile.
Optionally, the quality accounting of initiator described in the mixed slurry is 0.01%-2%.
In the present invention, gel-casting is used, so that work of the organic monomer in mixed slurry in crosslinking agent and initiator
It is cross-linked to form tridimensional network with lower, glass sand is dispersed therein and is not displaced in the curing process,
Crucible obtained is more stable.
Optionally, the solid concentration of the mixed slurry is greater than 90%wt.
It optionally, further include catalyst in the mixed slurry.Specifically, the catalyst can be, but not limited to as N, N,
N, N- tetramethylethylenediamine.
It optionally, further include dispersing agent in the mixed slurry.Further alternative, the dispersing agent includes organic poly- electricity
Solve at least one of matter and hyper-dispersant.Further optional, the dispersing agent includes polyacrylate, lignin sulfonic acid
At least one of salt, methylcellulose and citrate.
Optionally, the preparation process of the crucible body includes:
Quartz sand by purity no more than 99.9% is prepared into slurry, is prepared using injection forming or the method for infusing solidification forming
The crucible body.
Optionally, the crucible body include pedestal and by pedestal upwards derived from side wall.Further, described described
High purity quartz layer, the inner surface including the pedestal in the crucible body are formed on all or part of inner surface of crucible body
And/or high purity quartz layer is formed on the inner surface of the side wall.
Optionally, described that the mixed slurry is injected by the crucible body using gel-casting, it is cured to make the earthenware
High purity quartz layer is formed on all or part of inner surface of crucible ontology, comprising:
Internal model will be placed in the inner cavity of the crucible body, the mixed slurry is injected into the crucible body and described interior
It is cured that high purity quartz layer is formed on all or part of inner surface of the crucible body between mould.
Optionally, described that the mixed slurry is injected by the crucible body using gel-casting, it is cured to make the earthenware
High purity quartz layer is formed on all or part of inner surface of crucible ontology, comprising:
The mixed slurry is injected into the crucible body, is placing internal model, the cured whole in the crucible body
Or high purity quartz layer is formed on portion inner surface.
Further, internal model material includes stainless steel, tempered glass or heat-conducting silicon rubber.
It is further, described to inject the mixed slurry between the crucible body and the internal model, comprising:
By the way of pressure injection, the mixed slurry is injected between the crucible body and the internal model.
Further, the pressure is 0.1MPa-0.5MPa.Further, vacuum degree be (- 0.9) MPa- (-
0.5) pressure injection is carried out under MPa.
In the present invention, the size of the internal model is selected according to the thickness of the high purity quartz layer.
Optionally, the solidification includes at least one of water-bath solidification, electric heating solidification and microwave curing.
Optionally, the cured temperature is 50 DEG C -80 DEG C, curing time 10min-50min.
Optionally, the high purity quartz layer with a thickness of 0.1mm-20mm.
Optionally, the high purity quartz layer is equal thickness, progressive thickness or graded thickness.In the present invention, in polysilicon
During ingot casting, inner surface of crucible is longer in the time of the position contact silicon liquid close to bottom, and therefore, high purity quartz layer is close
The thickness that the thickness of inner surface of crucible bottom position is greater than close inner surface of crucible opening zone position is more advantageous to polycrystalline silicon ingot casting
When stop impurity infiltration, improve the purity of silicon ingot.
Optionally, the high purity quartz layer increases in the thickness of the estimated stops of silicon liquid level of solution, and the crucible body
Reduce in the thickness of the estimated stops of the silicon liquid level of solution, the thickness of the composite construction quartz ceramic crucible remains unchanged.
It optionally, further include sintering after the solidification.
Optionally, the roughening treatment include blasted rough, polish coarse or overstriking it is coarse.
Optionally, the roughness of the high purity quartz layer is 5 μm -50 μm.
Optionally, the composite construction quartz ceramic crucible with a thickness of 20mm-30mm.
It optionally, further include being dried before the roughening treatment.
It optionally, further include sintering, inspection, ultrasonic cleaning and drying after the roughening treatment.
In the present invention, the preparation process of the composite construction quartz ceramic crucible wants dust-proof, anti-pollution.
In the present invention, the crucible body inner surface can prepare high purity quartz layer described in multilayer, high-purity described in multilayer
Quartz layer is all made of the solidifying mode of note and is prepared, and the purity of the quartz sand in every layer of high purity quartz layer is uniform, described multiple
It is in rising trend by the purity of the quartz sand in every layer of structure of outer wall to inner surface to close structure quartz ceramic crucible.
Optionally, the surface of the high purity quartz layer is coated with silicon nitride layer.In the present invention, silicon nitride layer can be fine
In conjunction with high purity quartz layer, in polycrystal silicon ingot preparation process, do not have the infiltration of silicon nitride inclusions, there is no silicon nitrides to fall
The Hard Inclusion of the shortcomings that volt, silicon ingot not will increase, and be conducive to the application of silicon ingot.
In the present invention, the high purity quartz layer is formed for gel-casting, and by solidifying, being sintered, compactness improves, is anti-
Active reduction is answered, while being roughened rear adhesiveness and increasing, is conducive to adhere to silicon nitride layer, so that in polycrystal silicon ingot system
When standby, falling off and penetrating into silicon ingot, raising silicon ingot performance for silicon nitride layer is prevented.
Optionally, the bulk density of the composite construction quartz ceramic crucible is greater than 1.9g/cm3.It is further alternative, institute
The bulk density for stating composite construction quartz ceramic crucible is greater than 1.94g/cm3.In the present invention, the compactness of high purity quartz layer mentions
Height is conducive to prevent the impurity diffusion in crucible body into silicon ingot, and silicon ingot occurs without red side, improves the application value of silicon ingot.
The preparation method for the composite construction quartz ceramic crucible that second aspect of the present invention provides, by certain pure and partial size
High-purity stone of (purity is greater than 99.99%, and partial size is no more than 5mm and granular mass accounting of the partial size greater than 2mm is 10%-35%)
The mixed slurry of sand preparation is formed by curing high purity quartz on all or part of inner surface of crucible body by gel-casting
Layer, and then obtain composite construction quartz ceramic crucible.The reactivity of high purity quartz layer is effectively reduced in the preparation method, improves it
Compactness, and gel-casting can use the biggish glass sand of partial size, is less likely to occur to shift in the curing process, mention
The stability of high high purity quartz layer, to improve the stability of crucible.
Beneficial effects of the present invention:
The mixed slurry that the present invention is prepared using the glass sand of certain pure and partial size, by gel-casting in crucible
It is formed by curing high purity quartz layer on all or part of inner surface of ontology, by solidifying, being sintered, and then obtains composite construction quartz
Ceramic crucible improves the compactness of high purity quartz layer, effectively reduces the reactivity of high purity quartz layer, and barrier impurity expands
It dissipates, high purity quartz layer and silicon nitride layer adhesion improve, and in the curing process not using the biggish glass sand of partial size
The characteristics of being easily displaced improves the stability of high purity quartz layer and crucible entirety.The composite construction prepared through the invention
When quartz ceramic crucible carries out polycrystalline silicon ingot casting, it is possible to reduce impurity content and oxygen content in silicon ingot, the red side for reducing silicon ingot are existing
As obtaining the polycrystal silicon ingot of high quality.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described.Specific embodiment described herein is only used to explain this
Invention, is not intended to limit the present invention.
Fig. 1 is the structural schematic diagram of composite construction quartz ceramic crucible made from the embodiment of the present invention 1.
Fig. 2 is the structural schematic diagram of composite construction quartz ceramic crucible made from the embodiment of the present invention 2.
Fig. 3 is the structural schematic diagram of composite construction quartz ceramic crucible made from the embodiment of the present invention 3.
Fig. 4 is the structural schematic diagram of composite construction quartz ceramic crucible made from the embodiment of the present invention 4.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Embodiment 1
A kind of preparation method of composite construction quartz ceramic crucible, comprising:
The glass sand that purity is 99.99% and partial size is less than 5mm is taken, zirconia ball is added as grinding after being dissolved in water
Medium obtains quartz slurry, solid content 91%.Acrylamide, N,N methylene bis acrylamide and ammonium persulfate are added
Enter in above-mentioned quartz slurry, is uniformly mixed and obtains mixed slurry.
Crucible body is taken, tempered glass internal model is placed in the inner cavity of crucible body, is formed between internal model and crucible body
Type chamber.It moves back in above-mentioned mixed slurry injection type chamber in 60 DEG C of water-bath solidification 45min except internal model, makes using gel-casting
The inner surface for obtaining crucible body all adheres to one layer of high purity quartz layer, and composite construction quartz pottery is obtained after blasted rough is handled
Porcelain crucible, structure is as shown in Figure 1, composite construction quartz ceramic crucible includes crucible body 10 and is attached in crucible body 10
The high purity quartz layer 20 on surface.After measured, the composite construction quartz ceramic crucible with a thickness of 12mm, the thickness of high purity quartz layer
For 8mm, the bulk density of composite construction quartz ceramic crucible is 1.91g/cm3, inside surface roughness is 40 μm.
Embodiment 2
A kind of preparation method of composite construction quartz ceramic crucible, comprising:
Taking purity is 99.995% glass sand, wherein the coarse aggregate glass sand for being 1:2 containing mass ratio
Zirconia ball, nitridation is added after being dissolved in water in (partial size 0.5mm-5mm) and fine powder material glass sand (partial size is less than 0.5mm)
Silicon ball is ground in vertical ball mill as abrasive media, obtains quartz slurry, solid content 94%.By methyl-prop
Acrylamide, diisocyanate, azodiisobutyronitrile, azobisisoheptonitrile, N, N, N, N- tetramethylethylenediamine and polyacrylate
It is added in above-mentioned quartz slurry, is uniformly mixed and obtains mixed slurry, wherein the quality accounting of Methacrylamide is 0.5%, two
The quality accounting of isocyanates is the 3% of Methacrylamide quality, and the quality accounting of azodiisobutyronitrile is 0.5%, azo
The quality accounting of two different heptonitriles is 0.5%, N, N, N, and the quality accounting of N- tetramethylethylenediamine is 0.5%, polyacrylate
Quality accounting is 1%.
Crucible body is taken, using gel-casting, above-mentioned mixed slurry is injected into crucible sheet under the conditions of pressure is 0.1MPa
In the inner cavity of body, then stainless steel internal model is placed in crucible body inner cavity so that mixed slurry be placed in crucible body and internal model it
Between type chamber in, move back in 80 DEG C of electric heating solidification 10min except internal model, so that the inner surface of crucible body pedestal adheres to one layer of height
Pure quartz layer obtains composite construction quartz ceramic crucible after coarse processing of polishing, and structure is as shown in Fig. 2, composite construction
Quartz ceramic crucible includes crucible body 10 and the high purity quartz layer 20 for being attached to 10 base inner surface of crucible body.After measured,
The high purity quartz layer with a thickness of 5mm, the bulk density of composite construction quartz ceramic crucible is 1.92g/cm3, high purity quartz layer
Roughness is 35 μm.
Embodiment 3
A kind of preparation method of composite construction quartz ceramic crucible, comprising:
Taking purity is 99.9% glass sand, is fully ground in ball mill or blender after water is added, and be added
Organic polymer monomer, crosslinking agent and initiator prepare crucible body using gel-casting in crucible die.
Taking purity is 99.999% glass sand, wherein being made of by quality accounting following different-grain diameter particle:
25% partial size is greater than 2mm and is no more than the glass sand of 5mm, the glass sand of 10% partial size 1mm-2mm, 15% partial size
Not less than 0.5mm and less than the glass sand of 1mm, 5% partial size be greater than 0.1mm and glass sand less than 0.5mm,
Glass sand, 20% partial size of 25% partial size 0.05mm-0.1mm are less than the glass sand of 0.05mm, are dissolved in after water in batches
It is added in planetary ball mill, and uses alumina balls as abrasive media, obtain quartz slurry.By methylol acryloyl
Amine, divinylbenzene, azodiisobutyronitrile are added in above-mentioned quartz slurry, are uniformly mixed and obtain mixed slurry, wherein methylol
The quality accounting of acrylamide is 2%, and the quality accounting of divinylbenzene is the 3.5% of hydroxymethyl acrylamide quality, azo
The quality accounting of bis-isobutyronitrile is 0.1%.
Heat-conducting silicon rubber internal model is placed in the inner cavity of crucible body, shape forming cavity between internal model and crucible body.Using
Gel-casting, by above-mentioned mixed slurry injection type chamber under the conditions of pressure is 0.1MPa, vacuum degree is -0.6MPa, at 70 DEG C
Microwave curing 20min is moved back except internal model, so that crucible body side wall inner surfaces adhere to one layer of high purity quartz layer, it is coarse by overstriking
Composite construction quartz ceramic crucible is obtained after processing, structure is as shown in figure 3, composite construction quartz ceramic crucible includes crucible sheet
The thickness gradient of body 10 and the high purity quartz layer 20 for being attached to 10 base inner surface of crucible body, high purity quartz layer 20 increases, warp
Measurement, the bulk density of composite construction quartz ceramic crucible are 1.93g/cm3, high purity quartz bed roughness is 45 μm.
Embodiment 4
A kind of preparation method of composite construction quartz ceramic crucible, comprising:
Taking purity is that 99% glass sand is sufficiently mixed in ball mill or blender after water and binder is added
Slurry is made, using grouting process, crucible body is prepared in crucible die.
Taking purity is 99.995% glass sand, and zirconia ball, silicon nitride ball is added as grinding medium after being dissolved in water
Matter is ground in vertical ball mill, obtains the first quartz slurry.Methacrylamide, diisocyanate, azo two is different
Butyronitrile, N, N, N, N- tetramethylethylenediamine are added in above-mentioned quartz slurry, are uniformly mixed and obtain the first mixed slurry, wherein first
The quality accounting of base acrylamide is 0.5%, and the quality accounting of diisocyanate is the 2% of Methacrylamide quality, azo
The quality accounting of two different heptonitriles is 1%, N, N, N, and the quality accounting of N- tetramethylethylenediamine is 0.5%.
Heat-conducting silicon rubber internal model is placed in the inner cavity of crucible body, shape forming cavity between internal model and crucible body.Using
Gel-casting, by the first mixed slurry injection type chamber under the conditions of pressure is 0.3MPa, vacuum degree is -0.8MPa, at 50 DEG C
Microwave curing 45min is moved back except internal model, so that crucible body inner surface adheres to the first high purity quartz layer.
Take purity be 99.9999% glass sand, 56% partial size be greater than 2mm and no more than 5mm glass sand,
Glass sand, 8% partial size of 16% partial size 1mm-2mm is not less than 0.5mm and big less than glass sand, 6% partial size of 1mm
It is less than in 0.1mm and less than the glass sand of 0.5mm, the glass sand of 8% partial size 0.05mm-0.1mm, 6% partial size
The glass sand of 0.05mm is added agate ball, corundum ball as abrasive media after being dissolved in water, is ground in horizontal ball mill
Mill, obtains the second quartz slurry.By acrylamide, Methacrylamide, N,N methylene bis acrylamide, azo two different heptan
Nitrile, methylcellulose are added in above-mentioned quartz slurry, are uniformly mixed and obtain the second mixed slurry, wherein the quality of acrylamide
Accounting is 1%, and the quality accounting of Methacrylamide is 0.5%, N, and the quality accounting of N- methylene-bisacrylamide is
0.015%, the quality accounting of azobisisoheptonitrile is 3.5%, and the quality accounting of methylcellulose is 1%.
Using gel-casting, the injection of the second mixed slurry is attached with the first high purity quartz under the conditions of pressure is 0.1MPa
In the inner cavity of the crucible body of layer, then stainless steel internal model is placed in crucible body inner cavity, so that mixed slurry is placed in crucible sheet
It in type chamber between body and internal model, moves back in 65 DEG C of electric heating solidification 35min except internal model, so that crucible body inner surface attachment the
Two high purity quartz layers obtain composite construction quartz ceramic crucible after coarse processing of polishing, and structure is as shown in figure 4, compound
Structure quartz ceramic crucible includes crucible body 10 and the first high purity quartz layer 21 for being in turn attached to 10 inner surface of crucible body
With the second high purity quartz layer 22.After measured, the bulk density of composite construction quartz ceramic crucible is 1.92g/cm3, inner surface is thick
Rugosity is 50 μm.
The above is a preferred embodiment of the present invention, and but it cannot be understood as to the invention patent range
Limitation.It should be pointed out that for those skilled in the art, without departing from the principle of the present invention, also
Several improvements and modifications can be made, these modifications and embellishments are also considered to be within the scope of the present invention.
Claims (10)
1. a kind of composite construction quartz ceramic crucible, which is characterized in that the composite construction quartz ceramic crucible includes crucible sheet
Body and be arranged in the crucible body all or part of inner surface high purity quartz layer, the material packet of the high purity quartz layer
Purity is included greater than 99.99% and partial size is no more than the glass sand of 5mm, wherein partial size is greater than 2mm in the glass sand
Granular mass accounting be 10%-35%.
2. composite construction quartz ceramic crucible as described in claim 1, which is characterized in that described in the high purity quartz layer
Glass sand is bound up by the tridimensional network of the monomer crosslinked formation of organic polymer.
3. composite construction quartz ceramic crucible as described in claim 1, which is characterized in that the glass sand includes thick bone
Expect glass sand and fine powder material glass sand, coarse aggregate glass sand described in the high purity quartz layer and the fine powder
The mass ratio for expecting glass sand is 1:(1-4), the partial size of the coarse aggregate glass sand is 0.5mm-5mm, the fine powder
Expect that the partial size of glass sand is less than 0.5mm.
4. composite construction quartz ceramic crucible as claimed in claim 3, which is characterized in that the fine powder material glass sand is pressed
Quality accounting is made of following different-grain diameter particle:
Partial size is greater than 0.1mm and is less than 0.5mm 10%-30%
Partial size 0.05mm-0.1mm 30%-60%
Partial size is less than 0.05mm 30%-60%.
5. composite construction quartz ceramic crucible as claimed in claim 3, which is characterized in that the coarse aggregate glass sand is pressed
Quality accounting is made of following different-grain diameter particle:
Partial size is greater than 2mm and is no more than 5mm 50%-70%
Partial size 1mm-2mm 20%-40%
Partial size is not less than 0.5mm and is less than 1mm 10%-30%.
6. composite construction quartz ceramic crucible as described in claim 1, which is characterized in that the composite construction quartz-ceramics earthenware
The bulk density of crucible is greater than 1.9g/cm3。
7. composite construction quartz ceramic crucible as described in claim 1, which is characterized in that the roughness of the high purity quartz layer
It is 5 μm -50 μm, with a thickness of 0.1mm-20mm.
8. a kind of preparation method of composite construction quartz ceramic crucible characterized by comprising
By glass sand and water mixed grinding at quartz slurry, the purity of the glass sand is greater than 99.99% and partial size
No more than 5mm, wherein granular mass accounting of the partial size greater than 2mm is 10%-35% in the glass sand；To the stone
Organic polymer monomer, crosslinking agent and initiator are added in English slurry, is uniformly mixed and forms mixed slurry；
Crucible body is taken, the mixed slurry is injected by the crucible body using gel-casting, it is cured to make the crucible sheet
High purity quartz layer is formed on all or part of inner surface of body, roughened processing obtains composite construction quartz ceramic crucible.
9. the preparation method of composite construction quartz ceramic crucible as claimed in claim 8, which is characterized in that the mixed slurry
Described in organic polymer monomer quality accounting be 0.1%-5%, the quality accounting of crosslinking agent described in the mixed slurry
For the 0.1%-5% of the organic polymer monomer mass, the quality accounting of initiator described in the mixed slurry is
The solid concentration of 0.01%-2%, the mixed slurry are greater than 90%wt.
10. the preparation method of composite construction quartz ceramic crucible as claimed in claim 8, which is characterized in that the solidification packet
Include at least one of water-bath solidification, electric heating solidification and microwave curing, the cured temperature is 50 DEG C -80 DEG C, when solidification
Between be 10min-50min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811158982.1A CN109267150A (en) | 2018-09-30 | 2018-09-30 | A kind of composite construction quartz ceramic crucible and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811158982.1A CN109267150A (en) | 2018-09-30 | 2018-09-30 | A kind of composite construction quartz ceramic crucible and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109267150A true CN109267150A (en) | 2019-01-25 |
Family
ID=65195912
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811158982.1A Pending CN109267150A (en) | 2018-09-30 | 2018-09-30 | A kind of composite construction quartz ceramic crucible and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109267150A (en) |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101880166A (en) * | 2010-06-13 | 2010-11-10 | 洛阳北苑特种陶瓷有限公司 | Preparation method of large quartz ceramic crucible |
| CN102219360A (en) * | 2011-05-08 | 2011-10-19 | 江苏润弛太阳能材料科技有限公司 | Method for manufacturing polycrystalline silicon ingot casting fused quartz crucible without spraying |
| CN102219359A (en) * | 2011-04-06 | 2011-10-19 | 中材江苏太阳能新材料有限公司 | Method for forming large-size fused quartz ceramic crucible |
| CN102249523A (en) * | 2011-05-08 | 2011-11-23 | 江苏润弛太阳能材料科技有限公司 | Method for manufacturing spray-free fused quartz crucible for polycrystalline silicon cast ingot |
| CN102807312A (en) * | 2011-05-30 | 2012-12-05 | 比亚迪股份有限公司 | Crucible preparation method and crucible |
| CN102826737A (en) * | 2012-09-28 | 2012-12-19 | 常熟华融太阳能新型材料有限公司 | Quartz ceramic crucible for producing high-efficiency polycrystals and preparation method thereof |
| CN103359918A (en) * | 2012-04-01 | 2013-10-23 | 比亚迪股份有限公司 | Crucible and preparation method thereof |
| CN104860712A (en) * | 2015-04-14 | 2015-08-26 | 连云港浩特石英材料有限公司 | Method for preparing microporous lightweight thermal-insulation aggregate with waste fused quartz crucible |
| CN105541311A (en) * | 2015-12-09 | 2016-05-04 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method of silicon nitride-fused silica crucible for polysilicon ingot casting |
| CN107840647A (en) * | 2017-11-01 | 2018-03-27 | 烟台核晶陶瓷新材料有限公司 | A kind of fine and close high-purity layer preparation method of polycrystalline silicon ingot casting |
-
2018
- 2018-09-30 CN CN201811158982.1A patent/CN109267150A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101880166A (en) * | 2010-06-13 | 2010-11-10 | 洛阳北苑特种陶瓷有限公司 | Preparation method of large quartz ceramic crucible |
| CN102219359A (en) * | 2011-04-06 | 2011-10-19 | 中材江苏太阳能新材料有限公司 | Method for forming large-size fused quartz ceramic crucible |
| CN102219360A (en) * | 2011-05-08 | 2011-10-19 | 江苏润弛太阳能材料科技有限公司 | Method for manufacturing polycrystalline silicon ingot casting fused quartz crucible without spraying |
| CN102249523A (en) * | 2011-05-08 | 2011-11-23 | 江苏润弛太阳能材料科技有限公司 | Method for manufacturing spray-free fused quartz crucible for polycrystalline silicon cast ingot |
| CN102807312A (en) * | 2011-05-30 | 2012-12-05 | 比亚迪股份有限公司 | Crucible preparation method and crucible |
| CN103359918A (en) * | 2012-04-01 | 2013-10-23 | 比亚迪股份有限公司 | Crucible and preparation method thereof |
| CN102826737A (en) * | 2012-09-28 | 2012-12-19 | 常熟华融太阳能新型材料有限公司 | Quartz ceramic crucible for producing high-efficiency polycrystals and preparation method thereof |
| CN104860712A (en) * | 2015-04-14 | 2015-08-26 | 连云港浩特石英材料有限公司 | Method for preparing microporous lightweight thermal-insulation aggregate with waste fused quartz crucible |
| CN105541311A (en) * | 2015-12-09 | 2016-05-04 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method of silicon nitride-fused silica crucible for polysilicon ingot casting |
| CN107840647A (en) * | 2017-11-01 | 2018-03-27 | 烟台核晶陶瓷新材料有限公司 | A kind of fine and close high-purity layer preparation method of polycrystalline silicon ingot casting |
Non-Patent Citations (2)
| Title |
|---|
| 林宗寿等: "《无机非金属材料工学 第4版》", 31 December 2013, 武汉理工大学出版社 * |
| 陈大明等: "《先进陶瓷材料的注凝技术与应用》", 30 November 2011, 国防工业出版社 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP0891311B1 (en) | Tape cast silicon carbide dummy wafer | |
| CN112723875B (en) | Gallium oxide doped tin oxide ceramic target material and preparation method thereof | |
| CN111004034B (en) | Silicon carbide ceramic, method for producing same, and semiconductor component | |
| CN108911738B (en) | Porous barium titanate piezoelectric ceramic and preparation method thereof | |
| CN107935628A (en) | A kind of properties of SiC foam ceramics and preparation method thereof | |
| KR101530622B1 (en) | High performance Silica Blcok to be permeable water and manufacturing method thereof | |
| CN102300675A (en) | Grinding disk having plant seed capsules as a filler and method for the production thereof | |
| CN109267150A (en) | A kind of composite construction quartz ceramic crucible and preparation method thereof | |
| KR102124766B1 (en) | Plasma processing apparatus and manufacturing method of the same | |
| CN102432282A (en) | Method for manufacturing ITO (Indium Tin Oxide) target by gel injection molding technique | |
| CN116283251B (en) | Alumina ceramic and preparation method and application thereof | |
| JP2001158680A (en) | Silicon carbide-metal complex, method for producing the same, member for wafer-polishing device and table for wafer-polishing device | |
| JP2013095652A (en) | Silica sintered body crucible | |
| CN108558405A (en) | A kind of preparation method of high-compactness high-purity carborundum substrate material | |
| JP2001158674A (en) | Sintered compact of porous silicon carbide, method for producing the same, member for wafer-polishing device and table for wafer-polishing device | |
| JP4376479B2 (en) | Method for producing Si-SiC composite material | |
| KR102023972B1 (en) | Method for manufacturing large sized ceramics sintered body | |
| JP2002011653A (en) | Ceramic member and its manufacturing method, and table for wafer polishing device | |
| JP2002104884A (en) | Method of manufacturing ceramic member, method of manufacturing table for wafer polishing device | |
| JP2010076986A (en) | Method for producing pearlite | |
| CN101318818B (en) | Process for manufacturing high-purity niobium oxide, tantalum oxide ceramic crucible pot and manufactured products thereof | |
| JP4803877B2 (en) | Silicon carbide sintered body and method for producing the same | |
| CN115650759B (en) | Porous alumina ceramic sheet applied to gas sensor packaging and preparation method thereof | |
| JPH05229871A (en) | Production of ceramic sintered compact | |
| TW201040003A (en) | Mold for slip casting, method of using the same, and green and ITO target made thereby |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190125 |
|
| RJ01 | Rejection of invention patent application after publication |