CN103320854A - Coating structure for crucible, preparation method thereof, and crucible with coating structure - Google Patents

Coating structure for crucible, preparation method thereof, and crucible with coating structure Download PDF

Info

Publication number
CN103320854A
CN103320854A CN2013102262080A CN201310226208A CN103320854A CN 103320854 A CN103320854 A CN 103320854A CN 2013102262080 A CN2013102262080 A CN 2013102262080A CN 201310226208 A CN201310226208 A CN 201310226208A CN 103320854 A CN103320854 A CN 103320854A
Authority
CN
China
Prior art keywords
silicon
crucible
component
coating structure
inducing layer
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.)
Granted
Application number
CN2013102262080A
Other languages
Chinese (zh)
Other versions
CN103320854B (en
Inventor
苏春阳
张运锋
孟庆超
张任远
刘磊
潘明翠
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Yingli Group Co Ltd
Original Assignee
Yingli Group Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Yingli Group Co Ltd filed Critical Yingli Group Co Ltd
Priority to CN201310226208.0A priority Critical patent/CN103320854B/en
Publication of CN103320854A publication Critical patent/CN103320854A/en
Priority to PCT/CN2014/079207 priority patent/WO2014194832A1/en
Application granted granted Critical
Publication of CN103320854B publication Critical patent/CN103320854B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B11/00Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/002Crucibles or containers for supporting the melt
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02Elements
    • C30B29/06Silicon

Abstract

The invention provided a coating structure for a crucible, a preparation method thereof, and a crucible comprising the coating structure. The coating structure comprises an isolation layer and an induction layer. The isolation layer is covered on the surface of a crucible substrate. The induction layer is covered on the surface of the isolation layer. The coating structure adopts the double-layer structure with the isolation layer and the induction layer. With the induction layer, silicon melt crystal growth can be loaded, and silicon melt crystal growth effect can be promoted, such that polysilicon ingot quality can be ensured. With the isolation layer, the formed polysilicon ingot can be isolated from the crucible body, such that the impurities of the crucible body can be prevented from diffusing to the polysilicon ingot, and the crucible can be prevented from adhesion with the grown polysilicon ingot. Therefore, the polysilicon ingot can be smoothly de-molded. Also, the quality of the prepared polysilicon ingot can be ensured.

Description

Crucible is with coating structure, its preparation method and comprise its crucible
Technical field
The present invention relates to the casting field of polysilicon, in particular to a kind of crucible with coating structure, its preparation method and comprise its crucible.
Background technology
Polysilicon is the topmost starting material of solar cell, in the castingprocesses of polysilicon, usually adopt crucible as the long brilliant carrier of silicon melt, the smoothly demoulding in order to guarantee formed polycrystal silicon ingot not stick together with crucible, and prevent that the impurity in the crucible from spreading to silicon ingot, need to coating be set at crucible surface, existing crucible coating layer only is one deck silicon nitride layer usually.
In the castingprocesses of polysilicon, silicon melt begins forming core from the silicon nitride layer of crucible surface, and then long brilliant, and long brilliant process can be carried out along both direction, and the one, along the transverse growth that is parallel to silicon nitride layer, the 2nd, along the longitudinal growth perpendicular to silicon nitride layer.The contact angle of silicon melt and silicon nitride coating is larger, and the required condensate depression of forming core is high, simultaneously owing to there being Transverse Temperature Gradient, can cause behind the forming core transverse growth speed of nucleus higher.The longitudinal growth speed of nucleus then is subject to the inhibition of larger thermograde.This is just so that the polycrystal silicon ingot that forms at this silicon nitride coating, and grain shape obvious difference, size are uneven and in the majority with dendrite, has finally affected the quality of the polysilicon of casting.
Summary of the invention
The present invention aims to provide a kind of crucible with coating structure, its preparation method and comprises its crucible, to improve the quality with its polycrystal silicon ingot of being grown.
To achieve these goals, one aspect of the present invention provides a kind of crucible coating structure, and this coating structure is overlying on the crucible substrate surface, comprising: sealing coat is overlying on the surface of crucible base material; Inducing layer is overlying on the surface of sealing coat.
Further, described inducing layer comprises by weight: the first component of 50~300 parts and 50~300 parts second component, the first component is different from second component, and the first component is the material different with the silicon melt contact angle from second component.
Further, above-mentioned the first component and second component are selected from respectively the group that is comprised of silicon nitride, silicon carbide, silicon-dioxide and silicon.
Further, above-mentioned inducing layer also comprises by weight and is not less than 10 parts the 3rd component, and described the 3rd component is selected from one or both in silicon nitride, silicon carbide, silicon-dioxide, the silicon, and is different from described the first component and described second component.
Further, above-mentioned inducing layer is comprised of the first component and second component, and the first component is and the contact angle of the silicon melt material less than 90 °, and second component is and the contact angle of the silicon melt material greater than 90 °.
Further, the weight ratio of above-mentioned the first component and described second component is 1.5~2:1.
Further, above-mentioned inducing layer comprises 100 parts silicon nitride and 150 parts silicon-dioxide by weight.
Further, above-mentioned sealing coat is silicon nitride layer.
Simultaneously, another aspect of the present invention, a kind of preparation method of coating structure is provided, may further comprise the steps: step 1, insolated layer materials is mixed with the first solvent, form the first slurry after stirring, above-mentioned the first slurry is sprayed or brushes on the crucible substrate surface, after the drying, form above-mentioned sealing coat; Step 2, the inducing layer material is mixed with the second solvent, form the second slurry after stirring, above-mentioned the second slurry is sprayed or brushes on above-mentioned insulation surface, after the drying, form above-mentioned inducing layer.
Further, above-mentioned the first solvent is water, and above-mentioned the second solvent is dehydrated alcohol.
Simultaneously, another aspect of the present invention also provides a kind of crucible, is provided with above-mentioned coating structure.
Beneficial effect of the present invention: crucible coating structure provided by the present invention, its preparation method and comprise its crucible, adopt the bilayer structure of sealing coat and inducing layer, it is long brilliant with the carrying silicon melt by inducing layer is set, and the long brilliant effect of promotion silicon melt, guarantee the quality of polycrystal silicon ingot, by sealing coat is set formed polycrystal silicon ingot and crucible body are isolated to prevent that the intrinsic impurity of crucible from spreading to polycrystal silicon ingot, prevent crucible and the polycrystal silicon ingot adhesion of growing by the setting that utilizes sealing coat, make the smooth demoulding of polycrystal silicon ingot, and then guarantee the quality of prepared polycrystal silicon ingot.
Description of drawings
The Figure of description that consists of the application's a part is used to provide a further understanding of the present invention, and illustrative examples of the present invention and explanation thereof are used for explaining the present invention, do not consist of improper restriction of the present invention.In the accompanying drawings:
Fig. 1 shows a kind of schematic diagram of inducing the coating structure of the long crystalline substance of silicon melt according to the embodiment of the invention.
Embodiment
Need to prove, in the situation that do not conflict, embodiment and the feature among the embodiment among the application can make up mutually.Describe below with reference to the accompanying drawings and in conjunction with the embodiments the present invention in detail.
Term " with the same or analogous material of silicon crystalline structure " refers to that crystalline structure is the material of positive tetrahedron or tetrahedral structure in the present invention.
In a kind of typical embodiment of the present invention, a kind of crucible coating structure is provided, this coating structure 200 is overlying on the surface of crucible base material 100, and it comprises sealing coat 210 and inducing layer 220.Sealing coat 210 is overlying on the surface of crucible base material 100; Inducing layer 220 is overlying on the surface of sealing coat 210.
This coating structure provided by the present invention has comprised sealing coat 210 and inducing layer 220.Wherein inducing layer 220 can carry the long crystalline substance of silicon melt, and promotes the long brilliant effect of silicon melt, guarantees the quality of polycrystal silicon ingot; And sealing coat 210 can be with polycrystal silicon ingot and the isolation of crucible body, can prevent that so just the intrinsic impurity of crucible from spreading to polycrystal silicon ingot, in addition, sealing coat 210 can also prevent that crucible and the polycrystal silicon ingot of growing from sticking together, to guarantee the smooth demoulding of polycrystal silicon ingot, and then improve the quality of prepared polycrystal silicon ingot, for making sealing coat 210 can fully play the effect of isolation impurity and the assurance demoulding, need it to have certain thickness, preferred this thickness is 100~400um, and those skilled in the art also can set according to practical situation the occurrence of this thickness.
Preferably, above-mentioned crucible comprises the first component of 50~300 parts and 50~300 parts second component by weight with inducing layer in the coating structure 220, the first component is different from second component, and the first component and second component are the material different with the contact angle of silicon melt.In this inducing layer 220 structures, contain simultaneously two kinds of different materials, utilize different materials different from the contact angle of silicon melt, the different characteristic of condensate depression that forming core is required, so that silicon melt is according to condensate depression order from low to high, a plurality of location points in the inducing layer 220 are forming core and growing up successively, and then has guaranteed the integrity of nucleus shape.More preferably, in the first component and the second component one be silicon or with the same or analogous material of silicon crystalline structure, another is the material different from silicon crystalline structure.
Crucible of the present invention with the inducing layer 220 of coating structure in the first component and second component include but not limited to silicon nitride, silicon carbide, silicon-dioxide or silicon etc., wherein preferred the first component and second component are selected from respectively the group that is comprised of silicon nitride, silicon carbide, silicon-dioxide and silicon.Silicon nitride, silicon carbide, silicon-dioxide and silicon all are common materials, and larger with silicon melt contact angle difference, using wherein, the formed inducing layer 220 of bi-material can effectively increase the forming core point of growing in the brilliant process, and guarantee the integrity of nucleus shape, and then improve the quality of polycrystal silicon ingot.
Also comprise in the inducing layer 220 of above-mentioned crucible with coating structure being not less than 10 parts the 3rd component, above-mentioned the 3rd component is selected from one or both that are different from above-mentioned the first component and second component in silicon nitride, silicon carbide, silicon-dioxide, the silicon.In the inducing layer 220 that bi-material forms, further add the other materials that is different from the first component and second component, the inducing layer 220 that forms after the material mixing of number of different types, utilize the differing materials character different from the wettability of silicon melt, more nucleation site further is provided, the silicon melt forming core is disperseed, and silicon melt is grown up according to condensate depression order from low to high successively forming core in different positions, further guarantee the brilliant integrity of shape of nuclear, improved the quality of polycrystal silicon ingot.
Crucible of the present invention with coating structure in inducing layer 220 formed by the first component and second component, and the first component is and the contact angle of the silicon melt material less than 90 °, second component is and the contact angle of the silicon melt material greater than 90 °.Contain simultaneously two kinds of different materials, can realize silicon crystal at a plurality of location points successively forming core and grow up, and then guaranteed the integrity of nucleus shape, simultaneously, only adopt two kinds of different materials, avoid the forming core point quantity of the first forming core that is not suitable for producing because of ratio in many gradients nucleation process few, affected the problem of subsequent forming forming core quality.And with inducing layer 220 that silicon melt directly contacts in adopt with the silicon melt contact angle and differ larger bi-material, the easier forming core of silicon melt, and then quantity and the Uniform Dispersion of increase forming core point, a large amount of forming core points are grown up rapidly, this is just so that nucleus quantity is many in the polycrystal silicon ingot that generates, size is little, and then has guaranteed the quality of the polycrystal silicon ingot that generates.Preferably the weight ratio of the first component and described second component is 1.5~2:1.More preferably, the first component is silicon nitride, and second component is a kind of in silicon carbide, silicon-dioxide and the silicon.More preferably, above-mentioned inducing layer 220 comprises 100 parts silicon nitride and 150 parts silicon-dioxide by weight.
Preferably, above-mentioned sealing coat 210 is silicon nitride layer.Silicon nitride has very high chemical stability, does not react with molten silicon and quartz, and the preparation of high-purity silicon nitride is also comparatively easy.
Include but not limited to sealing coat and inducing layer at crucible provided by the invention in coating structure; except sealing coat and inducing layer; can also comprise other layers; as long as the lowest layer of coating structure is set to sealing coat; outermost layer is set to inducing layer and gets final product, and those skilled in the art can select according to concrete demand the kind of other each layers, as long as the lowest layer of coating structure is sealing coat; outermost layer is inducing layer, all belongs to protection scope of the present invention.
The present invention also provides a kind of preparation method of coating structure, in a concrete embodiment, the method may further comprise the steps: step 1, sealing coat 210 materials are mixed with the first solvent, form the first slurry after stirring, the first slurry is sprayed or brushes on crucible base material 100 surfaces, after the drying, form sealing coat 210; Step 2, inducing layer 220 materials are mixed with the second solvent, form the second slurry after stirring, with the spraying of the second slurry or brush on described sealing coat 210 surfaces, after the drying, form described inducing layer 220.
In above-mentioned preparation process, employed solvent need guarantee therein good dispersiveness of material, in order to form stable slurry, more preferably can remove and not introduce as far as possible by simple and easy method the safety solvent of other impurity, for example the organic solvent of water, ethanol, other volatile decomposition or their mixed solvent; Wherein, the first solvent is preferably water, and the second solvent is preferably dehydrated alcohol.Water is the minimum solvent of cost, with the silicon nitride layer material mixing, can form stable slurry after stirring; Absolute ethanol volatilizes is good, cost is lower and be innoxious solvent, with the material mixing of inducing layer, can form stable slurry after stirring.In addition, in the layoutprocedure of slurry, can also add other additives, for example be used for improving the strength of coating silicon sol, those skilled in the art can reasonably select according to preparation method provided by the invention the kind of additive.
In above-mentioned preparation process, selected drying mode includes but not limited to that nature dries, forced air drying and heat drying, above-mentioned naturally drying refers to each layer in the coating is exposed to 4-24h in the air, above-mentioned forced air drying refers to that with each layer in the coating be dry 2-12h in the air dry oven of 1-10m/s at wind speed respectively, and above-mentioned heat drying refers to the dry 1-8h under 30-1200 ℃ temperature respectively of each layer in the coating; The forming method of the coating that adopts comprises spraying method and spread coating, can also select other chemistry or physical method.
Spread coating is to use the brushing instrument one or more times slurry to be coated on crucible surface, spraying method is to use air pressure spray gun or other Spray painting tool to carry out the coating preparation, and those skilled in the art can be according to the different choice coating forming method of materials and concrete processing parameter.
The present invention also provides a kind of crucible, is provided with above-mentioned coating structure 200 in this crucible.This set has the crucible of above-mentioned coating structure 200, utilize the inducing layer 220 in the coating structure 200 to induce the silicon melt crystallization, promote the brilliant effect of length of silicon melt, guarantee the quality of polysilicon, utilize the sealing coat 210 in the coating structure that crucible body and polycrystal silicon ingot are kept apart, prevent that the impurity in the crucible from spreading to polycrystal silicon ingot, and utilize sealing coat 210 in the coating structure to prevent the adhesion of crucible and polycrystal silicon ingot, make the smooth demoulding of polycrystal silicon ingot, and then guaranteed the quality of polycrystal silicon ingot.This crucible is preferably quartz crucible, quartz crucible is a kind of crucible that is most widely used in the polysilicon castingprocesses at present, its main component is silicon-dioxide, can stable bond with the coating structure that provides among the present invention, guaranteed crucible structural stability in use.
Further specify the application's beneficial effect for example 1 below with reference to specific embodiment 1-9 and contrast:
Embodiment 1
The silicon nitride of isolating layer material: 375g.
The silicon nitride of inducing layer raw material: 50g (with the silicon melt contact angle greater than 90 °); The silicon-dioxide of 300g (with the silicon melt contact angle less than 90 °).
Crucible base: quartz crucible.
The method spare-crucible that provides among the present invention is provided, and it may further comprise the steps:
Step 1, isolating layer material being mixed with 1 premium on currency, is that the mechanical stirrer of 300-1000W stirs the slurry that forms sealing coat behind the 30min with power, and this slurry is brushed on the quartz crucible substrate surface, shelves 2h and carry out drying under 1000 ℃ high temperature;
Step 2, the inducing layer raw material is mixed with 1 liter of dehydrated alcohol, be that the mechanical stirrer of 300-1000W stirs the slurry that forms inducing layer behind the 30min with power, this slurry is brushed on above-mentioned insulation surface, at room temperature shelve 4h and naturally dry, form inducing layer the crucible that provides among the present invention is provided.
Embodiment 2
The silicon nitride of isolating layer material: 375g.
The silicon nitride of inducing layer raw material: 300g; The silicon-dioxide of 50g.
Crucible base: quartz crucible.
Preparation method: identical with embodiment 1.
Embodiment 3:
The silicon nitride of isolating layer material: 375g.
The silicon nitride of inducing layer raw material: 310g; The silicon-dioxide of 40g.
Crucible base: quartz crucible.
Preparation method: with embodiment 1.
Embodiment 4:
The silicon nitride of isolating layer material: 375g.
The silicon nitride of inducing layer raw material: 40g; The silicon-dioxide of 310g.
Crucible base: quartz crucible.
Preparation method: with embodiment 1.
Embodiment 5:
The silicon nitride of isolating layer material: 375g.
The silicon nitride of inducing layer raw material: 100g; The silicon-dioxide of 200g.
Crucible base: quartz crucible.
Preparation method: with embodiment 1.
Embodiment 6:
The silicon nitride of isolating layer material: 375g.
The silicon nitride of inducing layer raw material: 200g; The silicon-dioxide of 100g.
Crucible base: quartz crucible.
Preparation method: with embodiment 1.
Embodiment 7
The silicon nitride of isolating layer material: 375g.
The silicon nitride of inducing layer raw material: 100g; The silicon-dioxide of 150g
Crucible base: quartz crucible.
Preparation method: identical with embodiment 1.
Embodiment 8
The silicon nitride of isolating layer material: 375g.
The silicon nitride of inducing layer raw material: 100g; The silicon-dioxide of 150g; 50g silicon carbide.
Crucible base: quartz crucible.
Preparation method: identical with embodiment 1.
Embodiment 9
The silicon nitride of isolating layer material: 375g.
The silicon nitride of inducing layer raw material: 100g; The silicon-dioxide of 150g; 25g silicon carbide; 25g silicon.
Crucible base: quartz crucible.
Preparation method: identical with embodiment 1.
Comparative Examples 1:
Coating material: 375g silicon nitride.
Crucible base: quartz crucible.
The preparation method: coating material is mixed with 1 premium on currency, is that the mechanical stirrer of 300-1000W stirs the slurry that forms sealing coat behind the 30min with power, and this slurry is brushed on the quartz crucible substrate surface, shelves 2h and carry out drying under 1000 ℃ high temperature.
Test:
Test raw material: the same batch of silicon material that Wacker company sells
Testing method: the content of starting materials such as input in the prepared crucible in embodiment 1-9 and Comparative Examples 1, use identical casting technique casting polycrystalline silicon ingot, and get that silico briquette top, middle part, equal height position, bottom silicon chip carry out the test of silicon chip dislocation desity in the middle of the silicon ingot
Silicon chip dislocation desity testing method: adopt the mixing solutions of hydrofluoric acid and nitric acid to carry out acidifying optical polishing 3min silicon chip, the polishing fluid composition proportion is: V(HF(49%)): V(HNO 3(68%))=and 1:3,3-5 washed with de-ionized water of silicon chip after the polishing adopts Secco corrosive fluid etching 15min, and Secco corrosive fluid composition proportion is V(K 2Cr 2O 7Solution (0.15mol/L)): V(HF(49%)): the V(glacial acetic acid)=25:50:1, then the point of under 500 times magnification silicon chip surface being chosen 9 same positions according to the nine grids arrangement mode with opticmicroscope is observed and is taken pictures, adopt the dislocation desity on these photos of computer image processing technology analytical calculation, then get its mean value as the dislocation desity of this silicon chip.
Test result is as shown in table 1:
Table 1
? The average AD value in top Middle part average A D value Bottom average A D value Whole excellent average A D value
Embodiment 1 8.37E+05 9.46E+05 1.26E+06 1.01E+06
Embodiment 2 1.10E+06 1.01E+06 9.94E+05 1.03E+06
Embodiment 3 1.23E+06 1.41E+06 1.01E+06 1.22E+06
Embodiment 4 1.16E+06 1.11E+06 5.04E+05 9.25E+05
Embodiment 5 3.62E+05 7.01E+05 8.25E+05 6.29E+05
Embodiment 6 6.12E+05 8.18E+05 9.30E+05 7.87E+05
Embodiment 7 3.37E+05 6.37E+05 7.71E+05 5.82E+05
Embodiment 8 4.27E+05 6.94E+05 9.13E+05 6.78E+05
Embodiment 9 6.23E+05 8.92E+05 9.18E+05 8.11E+05
Comparative Examples 1 1.25E+06 1.60E+06 1.48E+06 1.44E+06
Data as shown in table 1 as can be known, adopt crucible coating layer structure provided by the invention, the defect concentration of prepared polycrystal silicon ingot will be much smaller than the defect concentration of the prepared polycrystal silicon ingot of the crucible that adopts single silicon nitride layer, show by at sealing coat inducing layer being set, can effectively guarantee perfection of crystal in the polycrystal silicon ingot, improve the quality of polycrystal silicon ingot.Meanwhile, the ratio of material can obtain than the prepared better perfection of crystal of polycrystal silicon ingot of inducing layer that adopts two or more materials to form in the inducing layer that the control bi-material forms.
Crucible coating structure provided by the present invention, comprise its crucible and preparation method thereof, adopt the bilayer structure of sealing coat and inducing layer, on the one hand, it is long brilliant with the carrying silicon melt by the inducing layer that is mixed by differing materials is set, and the long brilliant effect of promotion silicon melt, make formed nucleus quantity many, distribute wide, size is little and shape is complete, in the majority with equiax crystal, guaranteed the quality of polycrystal silicon ingot, on the other hand, by sealing coat is set formed polycrystal silicon ingot and crucible body are isolated to prevent that the intrinsic impurity of crucible from spreading to polycrystal silicon ingot, prevent crucible and the polycrystal silicon ingot adhesion of growing by the setting that utilizes sealing coat, make the smooth demoulding of polycrystal silicon ingot, and then guarantee the quality of prepared polycrystal silicon ingot.
The above is the preferred embodiments of the present invention only, is not limited to the present invention, and for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any modification of doing, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.

Claims (10)

1. crucible coating structure, described coating structure (200) is overlying on crucible base material (100) surface, it is characterized in that, comprising:
Sealing coat (210) is overlying on the surface of described crucible base material (100);
Inducing layer (220) is overlying on the surface of described sealing coat (210).
2. coating structure according to claim 1, it is characterized in that, described inducing layer (220) comprises by weight: the first component of 50~300 parts and 50~300 parts second component, described the first component is different from described second component, and described the first component is the material different with the silicon melt contact angle from described second component; Preferably, described the first component and described second component are selected from respectively the group that is comprised of silicon nitride, silicon carbide, silicon-dioxide and silicon.
3. coating structure according to claim 2, it is characterized in that, described inducing layer (220) also comprises by weight and is not less than 10 parts the 3rd component, described the 3rd component is selected from one or both in silicon nitride, silicon carbide, silicon-dioxide, the silicon, and is different from described the first component and described second component.
4. coating structure according to claim 2, it is characterized in that, described inducing layer (220) is comprised of the first component and second component, and described the first component is and the contact angle of the silicon melt material less than 90 °, and described second component is and the contact angle of the silicon melt material greater than 90 °.
5. coating structure according to claim 4 is characterized in that, the weight ratio of described the first component and described second component is 1.5~2:1.
6. coating structure according to claim 5 is characterized in that, described inducing layer (220) comprises 100 parts silicon nitride and 150 parts silicon-dioxide by weight.
7. each described coating structure in 6 according to claim 1 is characterized in that, described sealing coat (210) is silicon nitride layer.
8. the preparation method of each described coating structure in the claim 1 to 7 is characterized in that, may further comprise the steps:
Step 1, sealing coat (210) material is mixed with the first solvent, form the first slurry after stirring, described the first slurry is sprayed or brushes on crucible base material (100) surface, after the drying, form described sealing coat (210);
Step 2, inducing layer (220) material is mixed with the second solvent, form the second slurry after stirring, described the second slurry is sprayed or brushes on described sealing coat (210) surface, after the drying, form described inducing layer (220).
9. preparation method according to claim 8 is characterized in that, described the first solvent is water, and described the second solvent is dehydrated alcohol.
10. a crucible is characterized in that, is provided with each described coating structure (200) in the claim 1 to 7 in the described crucible.
CN201310226208.0A 2013-06-07 2013-06-07 Crucible coating structure, its preparation method and comprise its crucible Active CN103320854B (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
CN201310226208.0A CN103320854B (en) 2013-06-07 2013-06-07 Crucible coating structure, its preparation method and comprise its crucible
PCT/CN2014/079207 WO2014194832A1 (en) 2013-06-07 2014-06-05 Coating structure for crucible, fabrication method thereof, and crucible comprising same

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201310226208.0A CN103320854B (en) 2013-06-07 2013-06-07 Crucible coating structure, its preparation method and comprise its crucible

Publications (2)

Publication Number Publication Date
CN103320854A true CN103320854A (en) 2013-09-25
CN103320854B CN103320854B (en) 2016-03-02

Family

ID=49189884

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201310226208.0A Active CN103320854B (en) 2013-06-07 2013-06-07 Crucible coating structure, its preparation method and comprise its crucible

Country Status (2)

Country Link
CN (1) CN103320854B (en)
WO (1) WO2014194832A1 (en)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103628128A (en) * 2013-12-12 2014-03-12 英利集团有限公司 Crucible, production method of crucible and casting method of polycrystalline silicon ingot
WO2014194832A1 (en) * 2013-06-07 2014-12-11 英利能源(中国)有限公司 Coating structure for crucible, fabrication method thereof, and crucible comprising same
CN104630884A (en) * 2015-01-23 2015-05-20 东海晶澳太阳能科技有限公司 Seed crystal for full-molten efficient polycrystalline silicon ingot, as well as preparation method and application thereof
CN104711671A (en) * 2013-12-11 2015-06-17 徐州协鑫太阳能材料有限公司 Crucible coat structure, production method and crucible
CN104962991A (en) * 2015-05-26 2015-10-07 江苏润弛太阳能材料科技有限公司 Quartz crucible and production method thereof
CN107916451A (en) * 2017-12-15 2018-04-17 江苏润弛太阳能材料科技有限公司 One kind casting polysilicon exempts to spray crucible
CN109642341A (en) * 2016-05-18 2019-04-16 瑞科斯太阳能源私人有限公司 Silicon ingot growth crucible with patterning raised structures layer

Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101213328A (en) * 2005-07-01 2008-07-02 维苏维尤斯·克鲁斯布公司 Crucible for the crystallization of silicon
WO2008118023A1 (en) * 2007-03-26 2008-10-02 Elkem Solar As A coating composition for a mould
US20080295294A1 (en) * 2007-06-01 2008-12-04 Gt Solar Incorporated Processing of fine silicon powder to produce bulk silicon
CN201842894U (en) * 2010-09-16 2011-05-25 扬州华尔光电子材料有限公司 Composite coating quartz crucible for polycrystalline silicon ingot preparation
CN201857440U (en) * 2010-11-02 2011-06-08 上海普罗新能源有限公司 Crucible for purification and ingot casting of solar-grade polysilicon
US20120167817A1 (en) * 2010-12-30 2012-07-05 Bernhard Freudenberg Method and device for producing silicon blocks
CN102776561A (en) * 2012-04-01 2012-11-14 江西赛维Ldk太阳能高科技有限公司 Polycrystalline silicon ingot, preparation method of polycrystalline silicon ingot, polycrystalline silicon slice and crucible for polycrystalline silicon ingot casting
CN202671713U (en) * 2012-04-01 2013-01-16 江西赛维Ldk太阳能高科技有限公司 Crucible for polycrystalline silicon cast ingots
CN103014852A (en) * 2013-01-10 2013-04-03 韩华新能源科技有限公司 Casting method of efficient polycrystalline silicon ingot
CN103088417A (en) * 2013-01-22 2013-05-08 晶海洋半导体材料(东海)有限公司 High-efficiency crucible for polycrystal ingot casting and preparation method thereof

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102005050593A1 (en) * 2005-10-21 2007-04-26 Esk Ceramics Gmbh & Co. Kg Skim coat for making a durable hard coating on substrates, e.g. crucibles for melt-processing silicon, comprises silicon nitride particles and a binder consisting of solid nano-particles made by a sol-gel process
CN102400214A (en) * 2010-09-16 2012-04-04 扬州华尔光电子材料有限公司 Quartz crucible with composite coating layers for preparing polycrystalline silicon ingot
CN103102170B (en) * 2011-11-11 2014-12-03 浙江昱辉阳光能源有限公司 Crucible and preparation method thereof
CN103122479A (en) * 2011-11-21 2013-05-29 常州市万阳光伏有限公司 Combined crucible for preparing polycrystalline silicon ingot
CN103130512B (en) * 2011-11-25 2014-10-15 浙江昱辉阳光能源有限公司 Silicon nitride crucible and manufacture method thereof
CN103132141A (en) * 2011-12-05 2013-06-05 江苏协鑫硅材料科技发展有限公司 Coating composition of graphite equipment used for polycrystalline silicon ingot furnace
CN202717875U (en) * 2012-03-15 2013-02-06 阿特斯(中国)投资有限公司 Crucible for silicon ingot and preparation method of coating on inner side thereof
CN103320854B (en) * 2013-06-07 2016-03-02 英利集团有限公司 Crucible coating structure, its preparation method and comprise its crucible

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101213328A (en) * 2005-07-01 2008-07-02 维苏维尤斯·克鲁斯布公司 Crucible for the crystallization of silicon
WO2008118023A1 (en) * 2007-03-26 2008-10-02 Elkem Solar As A coating composition for a mould
US20080295294A1 (en) * 2007-06-01 2008-12-04 Gt Solar Incorporated Processing of fine silicon powder to produce bulk silicon
CN201842894U (en) * 2010-09-16 2011-05-25 扬州华尔光电子材料有限公司 Composite coating quartz crucible for polycrystalline silicon ingot preparation
CN201857440U (en) * 2010-11-02 2011-06-08 上海普罗新能源有限公司 Crucible for purification and ingot casting of solar-grade polysilicon
US20120167817A1 (en) * 2010-12-30 2012-07-05 Bernhard Freudenberg Method and device for producing silicon blocks
CN102776561A (en) * 2012-04-01 2012-11-14 江西赛维Ldk太阳能高科技有限公司 Polycrystalline silicon ingot, preparation method of polycrystalline silicon ingot, polycrystalline silicon slice and crucible for polycrystalline silicon ingot casting
CN202671713U (en) * 2012-04-01 2013-01-16 江西赛维Ldk太阳能高科技有限公司 Crucible for polycrystalline silicon cast ingots
CN103014852A (en) * 2013-01-10 2013-04-03 韩华新能源科技有限公司 Casting method of efficient polycrystalline silicon ingot
CN103088417A (en) * 2013-01-22 2013-05-08 晶海洋半导体材料(东海)有限公司 High-efficiency crucible for polycrystal ingot casting and preparation method thereof

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2014194832A1 (en) * 2013-06-07 2014-12-11 英利能源(中国)有限公司 Coating structure for crucible, fabrication method thereof, and crucible comprising same
CN104711671A (en) * 2013-12-11 2015-06-17 徐州协鑫太阳能材料有限公司 Crucible coat structure, production method and crucible
CN104711671B (en) * 2013-12-11 2017-08-25 徐州协鑫太阳能材料有限公司 Crucible coating layer structure, preparation method and crucible
CN103628128A (en) * 2013-12-12 2014-03-12 英利集团有限公司 Crucible, production method of crucible and casting method of polycrystalline silicon ingot
CN103628128B (en) * 2013-12-12 2016-06-15 英利集团有限公司 Crucible and preparation method thereof, polycrystal silicon ingot casting method
CN104630884A (en) * 2015-01-23 2015-05-20 东海晶澳太阳能科技有限公司 Seed crystal for full-molten efficient polycrystalline silicon ingot, as well as preparation method and application thereof
CN104962991A (en) * 2015-05-26 2015-10-07 江苏润弛太阳能材料科技有限公司 Quartz crucible and production method thereof
CN104962991B (en) * 2015-05-26 2018-04-17 江苏润弛太阳能材料科技有限公司 A kind of silica crucible and preparation method thereof
CN109642341A (en) * 2016-05-18 2019-04-16 瑞科斯太阳能源私人有限公司 Silicon ingot growth crucible with patterning raised structures layer
CN107916451A (en) * 2017-12-15 2018-04-17 江苏润弛太阳能材料科技有限公司 One kind casting polysilicon exempts to spray crucible

Also Published As

Publication number Publication date
WO2014194832A1 (en) 2014-12-11
CN103320854B (en) 2016-03-02

Similar Documents

Publication Publication Date Title
CN103320854B (en) Crucible coating structure, its preparation method and comprise its crucible
CN101423942B (en) Alkali etch solution and method for preparing monocrystalline silicon pile fabrics
CN104835723B (en) Form the composition and method of p-diffusion layer, and the method for preparing photovoltaic cell
JP2016531835A (en) Polycrystalline silicon wafer texturing additive and method of use thereof
CN103451728B (en) N-type crystalline silicon and preparation method thereof
CN206204475U (en) A kind of crucible used for polycrystalline silicon ingot casting
CN104711673A (en) Preparation method of polycrystalline silicon ingot
CN100506936C (en) High precision polishing liquid, preparation method and use thereof
CN103266355A (en) Etching agent for polycrystalline silicon wafer and etching method using etching agent
CN105040108A (en) Texture surface making method for polycrystalline silicon solar battery
CN102367572B (en) Sintering-free spraying method of polysilicon ingot crucible
CN102010186B (en) Low-temperature-sintered high-alumina porcelain and preparation method thereof
CN102409575A (en) Full degradable prime coat film of water transfer paper and production technology of prime coat film
CN106986554A (en) A kind of preparation method of ultra-pure coating quartz crucible
CN105063748B (en) A kind of polycrystalline cast ingot high efficient crucible and preparation method thereof
CN102191536A (en) Method for controlling crystallization and nucleation on crucible bottom when using directional solidification method to grow silicon crystal
CN101973760B (en) Method for reducing firing temperature of aluminum oxide ceramics
CN101891210A (en) Preparation method of nano silicon dioxide powder
CN104846436B (en) A kind of preparation method of ultra-pure quartz ceramic crucible
CN102826737B (en) Quartz ceramic crucible for producing high-efficiency polycrystals and preparation method thereof
CN104831348B (en) A kind of NdGaO3The processing method of single crystalline substrate
CN103396170B (en) The preparation method of crucible pot coating for polysilicon casting ingot and crucible
CN105088199A (en) Method for preparing VO2 nanometer film with surface orderly microstructure
CN109537047A (en) A kind of silicon material matching method improving monocrystalline quality
CN102712481A (en) Polycrystalline silicon for solar cell, and process for production thereof

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant