CN107904658A - A kind of reduction furnace inner wall preparation method of composite coating - Google Patents
A kind of reduction furnace inner wall preparation method of composite coating Download PDFInfo
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- CN107904658A CN107904658A CN201711202339.XA CN201711202339A CN107904658A CN 107904658 A CN107904658 A CN 107904658A CN 201711202339 A CN201711202339 A CN 201711202339A CN 107904658 A CN107904658 A CN 107904658A
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- silver
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- furnace inner
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/12—Production of homogeneous polycrystalline material with defined structure directly from the gas state
- C30B28/14—Production of homogeneous polycrystalline material with defined structure directly from the gas state by chemical reaction of reactive gases
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
- C23C8/20—Carburising
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Crystallography & Structural Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a kind of reduction furnace inner wall preparation method of composite coating, have toward inner wall in the reduction furnace of silver coating and be passed through the hot hydrogen containing carbonaceous gas, carbonaceous gas in hot hydrogen adsorbs on the surface of silver coating first, and then gas-solid boundary of the carbonaceous gas on silver coating surface decomposes and reaction and generates simple substance carbon, simple substance carbon further reacts with the silver in silver film generates silver carbide, and then forms the carbonization silver layer of densification in silver layer surface.The present invention is by using above-mentioned process, make reduction furnace inner wall silver/silver carbide composite coating that there is high heat reflectivity, high thermal stability, high-corrosion resistance, high flushing resistance, solve traditional reduction furnace inside coating there are the defects of, it is possible to achieve reduction furnace continuous-stable it is energy saving and ensure high purity polycrystalline silicon steady production.And the preparation method has that easy to operate, technique is simple, the advantage such as of low cost, it is possible to achieve large-scale application.
Description
Technical field
The present invention relates to production of polysilicon equipment technical field, and in particular to a kind of side for preparing reduction furnace inside coating
Method.
Background technology
Improved Siemens are the mainstream technologys for producing polysilicon in the world, its core equipment is reduction furnace, reduction furnace
Operation principle is by silicon-containing gas (common silicon-containing gas for trichlorosilane and silane) and hydrogen by energization high temperature silicon core
Mix gas reaction generation polysilicon and be deposited on silicon core, final product is deposited on the polysilicon on silicon core, and product is final
Produced in the form of polycrystalline silicon rod from reduction furnace.
, it is necessary to which the temperature of silicon rod is maintained at 1000 DEG C -1200 DEG C by electric energy heating in polysilicon production process, reduction furnace
Interior heat is delivered on stove inner wall by two ways, and one kind is high temperature silicon rod by radiant heat transfer by its heat transfer to also
On former stove inner wall, a kind of is that heated reacting gas is transferred heat on inner wall by convection current heat transfer.Polycrystalline silicon reducing furnace
Mainly made by austenitic stainless steel, if polycrystalline reduction furnace wall temperature is excessive, on the one hand can cause austenite stainless
Steel is pressure-resistant hydraulic performance decline and produce deformation problems；On the other hand the alloying element in austenitic stainless steel can be caused to escape, and then
Can polluted product and destruction stainless steel structure.Therefore usually taken away using the pressure-bearing cooling water being arranged in reduction furnace chuck through heat
Radiation and convection current are delivered to the heat of reduction furnace inner wall surface, reduction furnace wall temperature is maintained at less than 500 DEG C, according to system
Meter, the heat that pressure-bearing cooling water is taken away account for the 80% of reduction furnace power consumption.
Instantly, more by reduction furnace inner-wall spraying silver coating, using the excellent infrared reflecting performance of silver coating, to carry
High reduction furnace inner wall reduces the radiant heat transfer in reduction furnace, reaches the energy reduced inside reduction furnace to the reflectivity of infra-red radiation
Amount loss, finally realizes and the energy saving of process is reduced in polysilicon production process.At present, the main thermal jet of reduction furnace inner-wall spraying technology
Painting technology and cold spray technique, plasma spray technology are using specific that sprayed on material is heated to melting or semi-molten shape by heat source
State, then will melt by flame stream or working gas or the particle of semi-molten accelerates to after certain speed and sprays to base to be sprayed
Body surface face, forms a kind of technology of coating by the continuous pile up effect of particle.Cold spraying is to be accelerated with Laval-cavity nozzle through adding
The compressed gas of heat is used as working gas, and the carrier gas of high speed accelerates raw material powder to be sprayed from spray gun, with low temperature, high speed and complete
Reduction furnace inner wall is collided under solid-state, raw materials particles are deposited on inner wall after violent plastic deformation occurs at the same time with reduction furnace inner wall
Surface, and then the technology for the pile up effect formation coating for passing through particle.In the reduction furnace course of work, high temperature, corrosion in stove
Atmosphere, air scour and reduction furnace cleaning operation can destroy silver film, cause the fast dissipation of silver film or come off, single
Fine silver film layer there are the defects of limited to the development of reduction furnace power-saving technology, therefore, develop a kind of stable structure, have the high fever anti-
The reduction furnace inside coating of performance is penetrated, realizes that polycrystalline silicon reducing furnace continuous-stable is energy saving and the steady production of high purity polycrystalline silicon, is
The current problem for being badly in need of solving.
The content of the invention
The technical problem to be solved in the present invention is in view of the shortcomings of the prior art, there is provided a kind of stable structure, have heat instead
Penetrate performance, can solve the simple silver film of reduction furnace inner wall there are the defects of, realize polycrystalline silicon reducing furnace continuous-stable it is energy saving and
The reduction furnace inner wall preparation method of composite coating of high purity polycrystalline silicon steady production.
In order to solve the above technical problems, the present invention adopts the following technical scheme that：It is prepared by a kind of reduction furnace inner wall composite coating
Method, it is characterised in that：Have toward inner wall and the hot hydrogen containing carbonaceous gas is passed through in the reduction furnace of silver coating, in hot hydrogen
Carbonaceous gas adsorbs on the surface of silver coating first, and then gas-solid boundary of the carbonaceous gas on silver coating surface is decomposed instead
Simple substance carbon and should be generated, simple substance carbon further reacts with the silver in silver film generates silver carbide, and then in silver layer surface shape
Into fine and close carbonization silver layer, silver carbide is a kind of white compound of undefined structure, has high heat reflectivity, high heat stability
Property, high-corrosion resistance, high flushing resistance the advantages that, it is possible to achieve reduction furnace continuous-stable it is energy saving and ensure high purity polycrystalline silicon
Steady production.
Reduction furnace inner wall silver coating prepares the reduction furnace inner wall silver to form that thickness is 0.1mm-10mm by cold spray process
Coating.
Preferably, the carbonaceous gas is CxH2x+2, wherein x≤4, carbonaceous gas concretely methane.
Preferably, molar content of the carbonaceous gas in hot hydrogen is 0.5%-5%, and more preferably, carbonaceous gas is in hot hydrogen
Molar content in gas is 0.5%-1.2%.
Preferably, the operating temperature of the hot hydrogen containing carbonaceous gas is 100 DEG C -1000 DEG C, more preferably, contains carbon containing gas
The operating temperature of the hot hydrogen of body is 300 DEG C -900 DEG C.
Preferably, the operating pressure of the hot hydrogen containing carbonaceous gas is 0.3MPa-0.8MPa, more preferably, containing carbon containing
The operating pressure of the hot hydrogen of gas is 0.3MPa-0.6MPa, and most preferably, the operating pressure of the hot hydrogen containing carbonaceous gas is
0.5MPa-0.6MPa。
Preferably, silver carbide is controlled by the operating temperature and carbonaceous gas concentration that regulate and control the hot hydrogen containing carbonaceous gas
The thickness of layer, the thickness for making carbonization silver layer is 0.05mm-0.1mm.
The present invention makes reduction furnace inner wall silver/silver carbide composite coating have high heat reflection by using above-mentioned process
The advantages that rate, high thermal stability, high-corrosion resistance, high flushing resistance, solve existing for traditional reduction furnace inside coating
Defect, it is possible to achieve reduction furnace continuous-stable is energy saving and ensures the steady production of high purity polycrystalline silicon.And the preparation method has appearance
It is easy to operate, technique is simple, the advantage such as of low cost, it is possible to achieve large-scale application.
Embodiment
It is described further with reference to embodiment：
Embodiment 1
Have toward inner wall and the hot hydrogen containing carbonaceous gas is passed through in the reduction furnace of silver coating, the carbonaceous gas in hot hydrogen
Adsorb first on the surface of silver coating, and then gas-solid boundary of the carbonaceous gas on silver coating surface is decomposed and reaction and generated
Simple substance carbon, simple substance carbon further reacts with the silver in silver film generates silver carbide, and then forms densification in silver layer surface
Be carbonized silver layer, and silver carbide is a kind of white compound of undefined structure, has high heat reflectivity, high thermal stability, high corrosion resistant
The advantages that corrosion energy, high flushing resistance, it is possible to achieve reduction furnace continuous-stable is energy saving and ensures that stablizing for high purity polycrystalline silicon gives birth to
Production.
Reduction furnace inner wall silver coating is prepared by cold spray process, and it is 0.1mm to make reduction furnace inner wall silver coating thickness.
The carbonaceous gas is methane.
Molar content of the carbonaceous gas in hot hydrogen is 0.5%.
The operating temperature of the hot hydrogen containing carbonaceous gas is 600 DEG C.
The operating pressure of the hot hydrogen containing carbonaceous gas is 0.5MPa.
The thickness of carbonization silver layer is 0.05mm.
Embodiment 2
Have toward inner wall and the hot hydrogen containing carbonaceous gas is passed through in the reduction furnace of silver coating, the carbonaceous gas in hot hydrogen
Adsorb first on the surface of silver coating, and then gas-solid boundary of the carbonaceous gas on silver coating surface is decomposed and reaction and generated
Simple substance carbon, simple substance carbon further reacts with the silver in silver film generates silver carbide, and then forms densification in silver layer surface
Be carbonized silver layer, and silver carbide is a kind of white compound of undefined structure, has high heat reflectivity, high thermal stability, high corrosion resistant
The advantages that corrosion energy, high flushing resistance, it is possible to achieve reduction furnace continuous-stable is energy saving and ensures that stablizing for high purity polycrystalline silicon gives birth to
Production.
Reduction furnace inner wall silver coating is prepared by cold spray process, and it is 1mm to make reduction furnace inner wall silver coating thickness.
The carbonaceous gas is methane.
Molar content of the carbonaceous gas in hot hydrogen is 5%.
The operating temperature of the hot hydrogen containing carbonaceous gas is 800 DEG C.
The operating pressure of the hot hydrogen containing carbonaceous gas is 0.8MPa.
The thickness of the carbonization silver layer is 0.08mm.
Embodiment 3
Have toward inner wall and the hot hydrogen containing carbonaceous gas is passed through in the reduction furnace of silver coating, the carbonaceous gas in hot hydrogen
Adsorb first on the surface of silver coating, and then gas-solid boundary of the carbonaceous gas on silver coating surface is decomposed and reaction and generated
Simple substance carbon, simple substance carbon further reacts with the silver in silver film generates silver carbide, and then forms densification in silver layer surface
Be carbonized silver layer, and silver carbide is a kind of white compound of undefined structure, has high heat reflectivity, high thermal stability, high corrosion resistant
The advantages that corrosion energy, high flushing resistance, it is possible to achieve reduction furnace continuous-stable is energy saving and ensures that stablizing for high purity polycrystalline silicon gives birth to
Production.
Reduction furnace inner wall silver coating is prepared by cold spray process, and it is 0.5mm to make reduction furnace inner wall silver coating thickness.
The carbonaceous gas is methane.
Molar content of the carbonaceous gas in hot hydrogen is 1%.
The operating temperature of the hot hydrogen containing carbonaceous gas is 900 DEG C.
The operating pressure of the hot hydrogen containing carbonaceous gas is 0.3MPa.
The thickness of the carbonization silver layer is 0.1mm.
Embodiment 4
Have toward inner wall and the hot hydrogen containing carbonaceous gas is passed through in the reduction furnace of silver coating, the carbonaceous gas in hot hydrogen
Adsorb first on the surface of silver coating, and then gas-solid boundary of the carbonaceous gas on silver coating surface is decomposed and reaction and generated
Simple substance carbon, simple substance carbon further reacts with the silver in silver film generates silver carbide, and then forms densification in silver layer surface
Be carbonized silver layer, and silver carbide is a kind of white compound of undefined structure, has high heat reflectivity, high thermal stability, high corrosion resistant
The advantages that corrosion energy, high flushing resistance, it is possible to achieve reduction furnace continuous-stable is energy saving and ensures that stablizing for high purity polycrystalline silicon gives birth to
Production.
Reduction furnace inner wall silver coating is prepared by cold spray process, and it is 10mm to make reduction furnace inner wall silver coating thickness.
The carbonaceous gas is methane.
Molar content of the carbonaceous gas in hot hydrogen is 3%.
The operating temperature of the hot hydrogen containing carbonaceous gas is 100 DEG C.
The operating pressure of the hot hydrogen containing carbonaceous gas is 0.4MPa.
The thickness of the carbonization silver layer is 0.07mm.
Embodiment 5
Have toward inner wall and the hot hydrogen containing carbonaceous gas is passed through in the reduction furnace of silver coating, the carbonaceous gas in hot hydrogen
Adsorb first on the surface of silver coating, and then gas-solid boundary of the carbonaceous gas on silver coating surface is decomposed and reaction and generated
Simple substance carbon, simple substance carbon further reacts with the silver in silver film generates silver carbide, and then forms densification in silver layer surface
Be carbonized silver layer, and silver carbide is a kind of white compound of undefined structure, has high heat reflectivity, high thermal stability, high corrosion resistant
The advantages that corrosion energy, high flushing resistance, it is possible to achieve reduction furnace continuous-stable is energy saving and ensures that stablizing for high purity polycrystalline silicon gives birth to
Production.
Reduction furnace inner wall silver coating is prepared by cold spray process, and it is 8mm to make reduction furnace inner wall silver coating thickness.
The carbonaceous gas is methane.
Molar content of the carbonaceous gas in hot hydrogen is 1.2%.
The operating temperature of the hot hydrogen containing carbonaceous gas is 1000 DEG C.
The operating pressure of the hot hydrogen containing carbonaceous gas is 0.8MPa.
The thickness of the carbonization silver layer is 0.1mm.
The present invention is described in detail above, it is described above, it is only the preferred embodiments of the invention, when cannot
Limit the practical range of the present invention, i.e., it is all to make equivalent changes and modifications according to the application scope, it all should still belong to the present invention and cover model
In enclosing.
Claims (8)
- A kind of 1. reduction furnace inner wall preparation method of composite coating, it is characterised in that：Have toward inner wall in the reduction furnace of silver coating and lead to Enter the hot hydrogen containing carbonaceous gas, the carbonaceous gas in hot hydrogen adsorbs on the surface of silver coating, and then carbonaceous gas first Gas-solid boundary on silver coating surface, which is decomposed, reaction and generates simple substance carbon, simple substance carbon further with the silver hair in silver film Raw reaction generation silver carbide, and then the carbonization silver layer of densification is formed in silver layer surface, have high heat reflectivity, high thermal stability, The carbonization silver layer of high-corrosion resistance and high flushing resistance forms reduction furnace inner wall composite coating.
- 2. reduction furnace inner wall preparation method of composite coating according to claim 1, it is characterised in that：The silver of reduction furnace inner wall Coating is that the reduction furnace inner wall silver coating to form that thickness is 0.1mm-10mm is prepared by cold spray process.
- 3. reduction furnace inner wall preparation method of composite coating according to claim 2, it is characterised in that：The carbon containing gas Body is CxH2x+2, wherein x≤4.
- 4. reduction furnace inner wall preparation method of composite coating according to claim 3, it is characterised in that：The carbonaceous gas is Methane.
- 5. reduction furnace inner wall preparation method of composite coating according to claim 1, it is characterised in that：The carbonaceous gas exists Molar content in the hot hydrogen is 0.5%-5%.
- 6. reduction furnace inner wall preparation method of composite coating according to claim 1, it is characterised in that：It is described to contain carbon containing gas The operating temperature of the hot hydrogen of body is 100 DEG C -1000 DEG C.
- 7. reduction furnace inner wall preparation method of composite coating according to claim 1, it is characterised in that：It is described to contain carbon containing gas The operating pressure of the hot hydrogen of body is 0.3MPa-0.8MPa.
- 8. reduction furnace inner wall preparation method of composite coating according to claim 1, it is characterised in that：Contained by regulation and control The thickness of operating temperature and carbonaceous gas concentration the control carbonization silver layer of the hot hydrogen of carbon gas, the thickness for making carbonization silver layer are 0.05mm-0.1mm。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111286731A (en) * | 2020-02-20 | 2020-06-16 | 亚洲硅业(青海)股份有限公司 | Inner wall coating of polycrystalline silicon reduction furnace bell jar, preparation method of inner wall coating, spraying device of inner wall coating of polycrystalline silicon reduction furnace bell jar and application |
| CN111334788A (en) * | 2020-04-09 | 2020-06-26 | 亚洲硅业(青海)股份有限公司 | Coating of polycrystalline silicon reduction furnace, preparation method of coating, polycrystalline silicon reduction furnace and application of coating |
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| CN102674679A (en) * | 2011-03-14 | 2012-09-19 | 胡倾宇 | Polycrystalline silicon reduction furnace lining coating and production method thereof |
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| JP2001294416A (en) * | 2000-04-07 | 2001-10-23 | Mitsubishi Materials Polycrystalline Silicon Corp | Device for producing polycrystalline silicon |
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| CN102674679A (en) * | 2011-03-14 | 2012-09-19 | 胡倾宇 | Polycrystalline silicon reduction furnace lining coating and production method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111286731A (en) * | 2020-02-20 | 2020-06-16 | 亚洲硅业(青海)股份有限公司 | Inner wall coating of polycrystalline silicon reduction furnace bell jar, preparation method of inner wall coating, spraying device of inner wall coating of polycrystalline silicon reduction furnace bell jar and application |
| CN111286731B (en) * | 2020-02-20 | 2020-12-15 | 亚洲硅业(青海)股份有限公司 | Inner wall coating of polycrystalline silicon reduction furnace bell jar, preparation method of inner wall coating, spraying device of inner wall coating of polycrystalline silicon reduction furnace bell jar and application |
| CN111334788A (en) * | 2020-04-09 | 2020-06-26 | 亚洲硅业(青海)股份有限公司 | Coating of polycrystalline silicon reduction furnace, preparation method of coating, polycrystalline silicon reduction furnace and application of coating |
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Application publication date: 20180413 |