CN107252762A - A kind of spraying coating process of high-efficiency polycrystalline blowing crucible - Google Patents

A kind of spraying coating process of high-efficiency polycrystalline blowing crucible Download PDF

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Publication number
CN107252762A
CN107252762A CN201710339558.6A CN201710339558A CN107252762A CN 107252762 A CN107252762 A CN 107252762A CN 201710339558 A CN201710339558 A CN 201710339558A CN 107252762 A CN107252762 A CN 107252762A
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Prior art keywords
crucible
spraying
spray
powder
somebody
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Pending
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CN201710339558.6A
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Chinese (zh)
Inventor
张泽林
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NANTONG ZONGYI NOVEL MATERIALS Co Ltd
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NANTONG ZONGYI NOVEL MATERIALS Co Ltd
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Priority to CN201710339558.6A priority Critical patent/CN107252762A/en
Publication of CN107252762A publication Critical patent/CN107252762A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D3/00Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B05D3/02Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
    • B05D3/0218Pretreatment, e.g. heating the substrate
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D1/00Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
    • 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
    • C30B35/00Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
    • C30B35/002Crucibles or containers

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Metallurgy (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Ceramic Products (AREA)

Abstract

The invention discloses a kind of spraying coating process of high-efficiency polycrystalline blowing crucible, comprise the following steps:--- crucible heating --- --- stirring --- examination spray --- spraying --- cooling with powder that crucible is checked.Powder material spray silicon nitride is sprayed and painted on crucible surface by the crucible spraying in the present invention with pure water and silica gel; under heat effect; liquid nitrogen SiClx is set uniformly to adsorb crucible surface; form powdery coating; coating purpose is that protection silica crucible at high temperature with silicon isolate by silica crucible; liquid-state silicon is not reacted with silica crucible, and rupture silica crucible, and cold really rear final guarantee silicon heavy stone used as an anchor demoulding integrality.

Description

A kind of spraying coating process of high-efficiency polycrystalline blowing crucible
Technical field
The invention belongs to spraying coating process field, and in particular to a kind of spraying coating process of high-efficiency polycrystalline blowing crucible.
Background technology
Crucible spraying is to utilize to be different from other spraying technologies and method, and crucible spraying is that application crucible makes it by heating Liquefied mixture (silicon nitride) is attached to rapidly crucible surface.The method of application crucible can be divided into hot spraying and two kinds of sides of roller coating Method coating processes, but its technical matters of roller coating application is simple, and application coating is uneven, and the time is long, and silicon nitride usage amount is big, cost Height, so the present invention uses more advanced technique plasma spray technology.
Silicon nitride molecular formula is Si3N4, it is a kind of important structural ceramic material.It is a kind of superhard material, and itself has Lubricity, and it is wear-resistant;In addition to hydrofluoric acid, it not with other inorganic acid reactions, resistance to corrosion is strong, anti-oxidant during high temperature. And it can also resist cold shock, have and more than 1000 DEG C are heated in air, quick refrigeration is drastically heated again, also will not fragmentation.
The content of the invention
Goal of the invention:In order to solve the deficiencies in the prior art, the invention provides a kind of spray of high-efficiency polycrystalline blowing crucible Apply technique, it is to avoid crucible reacts with silicon material and the phenomenons such as overflow, viscous pot occurs;Optimization spraying coating process reduces making for silicon nitride Consumption, spraying is uniform, can reduce production cost.
Technical scheme:A kind of spraying coating process of high-efficiency polycrystalline blowing crucible, comprises the following steps:Crucible is checked --- crucible Heating --- --- stirring --- examination spray --- spraying --- cooling with powder;Wherein:
In the crucible heating:Crucible heating-up temperature is constant at 80 ± 2 DEG C;
It is described to match somebody with somebody in powder:The article of following species is configured by the proportioning of quality:Silicon nitride powder is 500-700 parts, and DI water is used Measure as 1400-1600 parts, Ludox is 100-300 parts;
In the stirring:Measure DI water and Ludox with specified volume in powder step with measuring cup to be stirred, stirring speed Spend and turn/min for 500-600, mixing time is 3-8min, is stirred;Then the nitridation for matching somebody with somebody predetermined weight in powder step is added Silica flour, stirs 8-13min at a same speed;
In the examination spray:Spray gun pressure scope is 25psi-35psi, spray is first tried on cardboard, when the liquid of injection is in paper In uniform vaporific distribution on plate, width shows that spray gun can be used for formal spraying in 3-5cm;
In the spraying:Sprayed surface vertical range needed for spray gun separation is 30-40cm, and positioning land crucible width is 15-20cm, by crossing condition even application anyhow, treats that bottom is done rear and sprayed again second time, is once sprayed in spraying process Thickness control is applied in less than 0.01mm, crucible spraying temperature is at 40 DEG C -65 DEG C.
It is used as optimization:It is described to match somebody with somebody in powder:The article of following species is configured by the proportioning of quality:Silicon nitride powder is 600 parts, DI water consumptions are 1500 parts, and Ludox is 200 parts.
It is used as optimization:In the stirring:DI water and Ludox with specified volume in powder step is measured with measuring cup to be stirred Mix, mixing speed is 550 turns/min, and mixing time is 5min, is stirred;Then the nitrogen for matching somebody with somebody predetermined weight in powder step is added SiClx powder, stirs 10min at a same speed.
It is used as optimization:In the examination spray:Spray gun pressure scope is 30psi, spray is first tried on cardboard, when the liquid of injection exists In uniform vaporific distribution on cardboard, width shows that spray gun can be used for formal spraying in 4cm.
It is used as optimization:In the spraying:Sprayed surface vertical range needed for spray gun separation is 35cm, positions land crucible Width is 18cm, by crossing condition even application anyhow, treats that bottom does rear and sprays second time again, in spraying process once Coating thickness is controlled in less than 0.01mm, and crucible spraying temperature is at 55 DEG C.
Beneficial effect:Powder material spray silicon nitride is sprayed and painted on crucible table by the crucible spraying in the present invention with pure water and silica gel Face, under heat effect, makes liquid nitrogen SiClx uniformly adsorb crucible surface, forms powdery coating, and coating purpose is protection stone English crucible at high temperature with silicon isolate by silica crucible, liquid-state silicon is not reacted with silica crucible, and ruptures silica crucible, and cold It is final after really to ensure silicon heavy stone used as an anchor demoulding integrality.
Wherein, silicon nitride is sprayed on using pure water and silica gel the inner surface of crucible, makes its absorption in crucible internal walls and bottom, Isolate crucible and silicon material during ingot casting, it is to avoid crucible reacts with silicon material and the phenomenons such as overflow, viscous pot occurs.
The present invention is that the silicon liquid coating that will be prepared is sprayed with the compressed air of purification, and spray gun pressure is 25psi- 35psi, spray distance is 30-40cm, and positioning land crucible width is 15-20cm, general in spraying process once to spray thickness Easily there is silicon in heating process in less than 0.01mm, otherwise and splits foaming pin holes etc. in degree control, and crucible spraying temperature is 40 In DEG C of -65 DEG C controls.
Embodiment
The technical scheme in the embodiment of the present invention will be clearly and completely described below, so that the technology of this area Personnel can be better understood from advantages and features of the invention, so as to make apparent boundary to protection scope of the present invention It is fixed.Embodiment described in the invention is only a part of embodiment of the invention, rather than whole embodiments, based on the present invention In embodiment, the every other implementation that those of ordinary skill in the art are obtained on the premise of creative work is not made Example, belongs to the scope of protection of the invention.
Specific embodiment 1
A kind of spraying coating process of high-efficiency polycrystalline blowing crucible, comprises the following steps:Crucible checks --- crucible heating --- --- stirring --- examination spray --- spraying --- cooling with powder;Wherein:
In the crucible heating:Crucible heating-up temperature is constant at 78 DEG C;
It is described to match somebody with somebody in powder:The article of following species is configured by the proportioning of quality:Silicon nitride powder is 500 parts, and DI water consumptions are 1400 parts, Ludox is 100 parts;
In the stirring:Measure DI water and Ludox with specified volume in powder step with measuring cup to be stirred, stirring speed Spend for 500 turns/min, mixing time is 3min, is stirred;Then the silicon nitride powder for matching somebody with somebody predetermined weight in powder step is added, with Same speed stirring 8min;
In the examination spray:Spray gun pressure scope is 25psi, spray is first tried on cardboard, when the liquid of injection is on cardboard Uniform vaporific distribution, width shows that spray gun can be used for formal spraying in 3cm;
In the spraying:Sprayed surface vertical range needed for spray gun separation is 30cm, and positioning land crucible width is 15cm, by crossing condition even application anyhow, treats that bottom is done rear and sprayed again second time, is once sprayed in spraying process thick Degree control is in less than 0.01mm, and crucible spraying temperature is at 40 DEG C.
Specific embodiment 2
A kind of spraying coating process of high-efficiency polycrystalline blowing crucible, comprises the following steps:Crucible checks --- crucible heating --- --- stirring --- examination spray --- spraying --- cooling with powder;Wherein:
In the crucible heating:Crucible heating-up temperature is constant at 82 DEG C;
It is described to match somebody with somebody in powder:The article of following species is configured by the proportioning of quality:Silicon nitride powder is 500-700 parts, and DI water is used Measure as 1600 parts, Ludox is 300 parts;
In the stirring:Measure DI water and Ludox with specified volume in powder step with measuring cup to be stirred, stirring speed Spend for 600 turns/min, mixing time is 8min, is stirred;Then the silicon nitride powder for matching somebody with somebody predetermined weight in powder step is added, with Same speed stirring 13min;
In the examination spray:Spray gun pressure scope is 35psi, spray is first tried on cardboard, when the liquid of injection is on cardboard Uniform vaporific distribution, width shows that spray gun can be used for formal spraying in 5cm;
In the spraying:Sprayed surface vertical range needed for spray gun separation is 40cm, and positioning land crucible width is 20cm, by crossing condition even application anyhow, treats that bottom is done rear and sprayed again second time, is once sprayed in spraying process thick Degree control is in less than 0.01mm, and crucible spraying temperature is at 65 DEG C.
Specific embodiment 3
A kind of spraying coating process of high-efficiency polycrystalline blowing crucible, comprises the following steps:Crucible checks --- crucible heating --- --- stirring --- examination spray --- spraying --- cooling with powder;Wherein:
In the crucible heating:Crucible heating-up temperature is constant at 80 DEG C;
It is described to match somebody with somebody in powder:The article of following species is configured by the proportioning of quality:Silicon nitride powder is 600 parts, and DI water consumptions are 1500 parts, Ludox is 200 parts;
In the stirring:Measure DI water and Ludox with specified volume in powder step with measuring cup to be stirred, stirring speed Spend for 550 turns/min, mixing time is 5min, is stirred;Then the silicon nitride powder for matching somebody with somebody predetermined weight in powder step is added, with Same speed stirring 10min;
In the examination spray:Spray gun pressure scope is 30psi, spray is first tried on cardboard, when the liquid of injection is on cardboard Uniform vaporific distribution, width shows that spray gun can be used for formal spraying in 4cm;
In the spraying:Sprayed surface vertical range needed for spray gun separation is 35cm, and positioning land crucible width is 18cm, by crossing condition even application anyhow, treats that bottom is done rear and sprayed again second time, is once sprayed in spraying process thick Degree control is in less than 0.01mm, and crucible spraying temperature is at 55 DEG C.
The present invention is that the silicon liquid coating that will be prepared is sprayed with the compressed air of purification, and spray gun pressure is 25psi- 35psi, spray distance is 30-40cm, and positioning land crucible width is 15-20cm, general in spraying process once to spray thickness Easily there is silicon in heating process in less than 0.01mm, otherwise and splits foaming pin holes etc. in degree control, and crucible spraying temperature is 40 In DEG C of -65 DEG C controls.
Powder material spray silicon nitride is sprayed and painted on crucible surface by the crucible spraying in the present invention with pure water and silica gel, is made in heating Under, liquid nitrogen SiClx is uniformly adsorbed crucible surface, form powdery coating, coating purpose is protection silica crucible in high temperature Lower silica crucible is isolated with silicon, liquid-state silicon is not reacted with silica crucible, and ruptures silica crucible, and cold really rear final guarantee Silicon heavy stone used as an anchor demoulding integrality.Wherein, silicon nitride is sprayed on using pure water and silica gel the inner surface of crucible, makes its absorption in crucible internal walls And bottom, crucible and silicon material are isolated during ingot casting, it is to avoid crucible reacts with silicon material and overflow, viscous pot etc. occurs now As.

Claims (5)

1. a kind of spraying coating process of high-efficiency polycrystalline blowing crucible, it is characterised in that:Comprise the following steps:Crucible is checked --- crucible Heating --- --- stirring --- examination spray --- spraying --- cooling with powder;Wherein:
In the crucible heating:Crucible heating-up temperature is constant at 80 ± 2 DEG C;
It is described to match somebody with somebody in powder:The article of following species is configured by the proportioning of quality:Silicon nitride powder is 500-700 parts, and DI water consumptions are 1400-1600 parts, Ludox is 100-300 parts;
In the stirring:Measure DI water and Ludox with specified volume in powder step with measuring cup to be stirred, mixing speed is 500-600 turns/min, and mixing time is 3-8min, is stirred;Then the silicon nitride powder for matching somebody with somebody predetermined weight in powder step is added, 8-13min is stirred at a same speed;
In the examination spray:Spray gun pressure scope is 25psi-35psi, spray is first tried on cardboard, when the liquid of injection is on cardboard In uniform vaporific distribution, width shows that spray gun can be used for formal spraying in 3-5cm;
In the spraying:Sprayed surface vertical range needed for spray gun separation is 30-40cm, and positioning land crucible width is 15- 20cm, by crossing condition even application anyhow, treats that bottom is done rear and sprayed again second time, is once sprayed in spraying process thick Degree control is in less than 0.01mm, and crucible spraying temperature is at 40 DEG C -65 DEG C.
2. the spraying coating process of high-efficiency polycrystalline blowing crucible according to claim 1, it is characterised in that:It is described to match somebody with somebody in powder:Press The article of the following species of proportioning configuration of quality:Silicon nitride powder is 600 parts, and DI water consumptions are 1500 parts, and Ludox is 200 parts.
3. the spraying coating process of high-efficiency polycrystalline blowing crucible according to claim 1, it is characterised in that:In the stirring:With Measuring cup measures DI water and Ludox with specified volume in powder step and is stirred, and mixing speed is 550 turns/min, mixing time For 5min, stir;Then the silicon nitride powder for matching somebody with somebody predetermined weight in powder step is added, 10min is stirred at a same speed.
4. the spraying coating process of high-efficiency polycrystalline blowing crucible according to claim 1, it is characterised in that:In the examination spray:Spray Rifle pressure limit is 30psi, and spray is first tried on cardboard, and when the liquid of injection is in uniform vaporific distribution on cardboard, width exists 4cm, shows that spray gun can be used for formal spraying.
5. the spraying coating process of high-efficiency polycrystalline blowing crucible according to claim 1, it is characterised in that:In the spraying:Spray Sprayed surface vertical range needed for rifle separation is 35cm, and positioning land crucible width is 18cm, equal by crossing condition anyhow Even spraying, treats that bottom is done rear and sprayed again second time, a coating thickness control is in less than 0.01mm in spraying process, earthenware Crucible spraying temperature is at 55 DEG C.
CN201710339558.6A 2017-05-15 2017-05-15 A kind of spraying coating process of high-efficiency polycrystalline blowing crucible Pending CN107252762A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107876362A (en) * 2017-11-10 2018-04-06 江苏协鑫硅材料科技发展有限公司 The automatic spraying process and crucible of large scale crucible for casting ingots coating

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102728532A (en) * 2012-06-29 2012-10-17 宜昌南玻硅材料有限公司 Method for preparing crucible sintering-free coating for polycrystalline silicon cast ingots
CN103506263A (en) * 2011-12-30 2014-01-15 英利能源(中国)有限公司 Polycrystalline silicon crucible spraying method free of drying and silicon nitride coating

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103506263A (en) * 2011-12-30 2014-01-15 英利能源(中国)有限公司 Polycrystalline silicon crucible spraying method free of drying and silicon nitride coating
CN102728532A (en) * 2012-06-29 2012-10-17 宜昌南玻硅材料有限公司 Method for preparing crucible sintering-free coating for polycrystalline silicon cast ingots

Non-Patent Citations (1)

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Title
百度文库: "坩埚喷涂作业指导书", 《HTTPS://WENKU.BAIDU.COM/VIEW/ABBCB2BCFAB069DC5122011D.HTML》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107876362A (en) * 2017-11-10 2018-04-06 江苏协鑫硅材料科技发展有限公司 The automatic spraying process and crucible of large scale crucible for casting ingots coating

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Application publication date: 20171017