CN114702848A - Coating slurry for graphite crucible and preparation and application methods thereof - Google Patents

Coating slurry for graphite crucible and preparation and application methods thereof Download PDF

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Publication number
CN114702848A
CN114702848A CN202210248159.XA CN202210248159A CN114702848A CN 114702848 A CN114702848 A CN 114702848A CN 202210248159 A CN202210248159 A CN 202210248159A CN 114702848 A CN114702848 A CN 114702848A
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CN
China
Prior art keywords
graphite crucible
coating slurry
parts
vanadium
aluminum alloy
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Pending
Application number
CN202210248159.XA
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Chinese (zh)
Inventor
李兰杰
万贺利
王方
王新东
徐峰
张旭
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Hegang Chengde Vanadium Titanium New Material Co ltd
HBIS Co Ltd Chengde Branch
Original Assignee
Hegang Chengde Vanadium Titanium New Material Co ltd
HBIS Co Ltd Chengde Branch
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Application filed by Hegang Chengde Vanadium Titanium New Material Co ltd, HBIS Co Ltd Chengde Branch filed Critical Hegang Chengde Vanadium Titanium New Material Co ltd
Priority to CN202210248159.XA priority Critical patent/CN114702848A/en
Publication of CN114702848A publication Critical patent/CN114702848A/en
Pending legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING 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
    • C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
    • C09D1/10—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances lime
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
    • C22C27/02—Alloys based on vanadium, niobium, or tantalum
    • C22C27/025—Alloys based on vanadium, niobium, or tantalum alloys based on vanadium

Abstract

The invention relates to the technical field of vanadium-aluminum alloy smelting, in particular to a coating slurry for a graphite crucible and a preparation and application method thereof, wherein the coating slurry for the graphite crucible comprises the following raw materials in parts by weight: calcium aluminate slag: 5-20 parts of quicklime: 50-100 parts of magnesium chloride: 2-50 parts of deionized water: 150-500 parts. The coating slurry for the graphite crucible can greatly reduce the contact probability of the graphite crucible and the alloy at high temperature, is not easy to melt, can not increase the content of carbon impurities in the alloy even if the coating slurry is melted, can obviously reduce the content of the carbon impurities in the vanadium-aluminum alloy, can prolong the service life of the graphite crucible and reduce the production cost.

Description

Coating slurry for graphite crucible and preparation and application methods thereof
Technical Field
The invention relates to the technical field of vanadium-aluminum alloy smelting, in particular to coating slurry for a graphite crucible and preparation and application methods thereof.
Background
The traditional method for producing vanadium-aluminum alloy is mainly a self-propagating method, a graphite crucible is used as a reactor in the self-propagating method, and slag and alloy inevitably contact with the bottom and the side wall of the graphite crucible in the production process. As the aluminothermic reduction reaction is carried out spontaneously, a large amount of heat is released instantly in the reaction process, slag and alloy are easy to splash, and partial loose carbon on the graphite crucible can be brought into the slag and the alloy in the splashing process, so that the content of carbon impurities in the vanadium-aluminum alloy is increased finally. Based on the above factors, the service cycle of the graphite crucible can be inevitably shortened, or the influence of the graphite crucible on the carbon content in the vanadium-aluminum alloy can be reduced by a method of timely replacing the graphite crucible after the surface smoothness is reduced when the obvious burning loss of the graphite crucible is found, so that the waste of the graphite crucible is greatly caused, the production cost is improved, and the effect of reducing the carbon impurity content in the vanadium-aluminum alloy is very slight.
Disclosure of Invention
In view of this, the application provides a coating slurry for a graphite crucible, which can greatly reduce the contact probability between the graphite crucible and an alloy at high temperature, and the coating slurry is not easy to melt, and even if the coating slurry is melted, the content of carbon impurities in the alloy cannot be increased, so that the content of carbon impurities in a vanadium-aluminum alloy can be obviously reduced, the service life of the graphite crucible can be prolonged, the production cost is reduced, and the defects of the prior art are overcome.
In order to achieve the purpose, the invention adopts the following technical scheme:
the application provides a coating slurry for a graphite crucible, which comprises the following raw materials in parts by weight: calcium aluminate slag: 5-20 parts of quicklime: 50-100 parts of magnesium chloride: 2-50 parts and deionized water: 150-500 parts.
According to the scheme shown in the embodiment of the application, the calcium aluminate slag used in the coating slurry of the graphite crucible has the characteristics of low impurity content, high hardness and high melting point, can be used as one of the coating slurries, can remarkably improve the high temperature resistance of the coating slurry, and is high in melting point and not easy to melt, so that the calcium aluminate slag cannot be doped in the alloy; the calcium oxide can be combined with the byproduct alumina to generate calcium aluminate in the high-temperature aluminothermic reduction reaction, so that the calcium oxide is used as the main raw material of the coating slurry, not only can new impurities be prevented from being introduced, but also the slag components in the vanadium-aluminum alloy smelting process can be improved; the magnesium chloride can improve the viscosity of the coating slurry, improve the adhesion degree of the coating slurry and the graphite crucible, and simultaneously has small influence on the components of the alloy and the slag in the high-temperature aluminothermic reduction process. The application provides a coating ground paste for graphite crucible can reduce graphite crucible and alloy contact probability under high temperature widely, can effectively completely cut off air and graphite crucible to the pollution of alloy under high temperature 1600-.
In combination with the first aspect, the calcium aluminate slag is a byproduct obtained by smelting vanadium-aluminum alloy.
The application provides a coating ground paste for graphite crucible uses the solid useless of self production as the raw materials, when reduction in production cost, has also reduced the emission of solid useless, has reduced environmental pollution.
With reference to the first aspect, the mass percentage content of CaO in the quicklime is greater than or equal to 95%, and the mass percentage content of Fe in the quicklime is greater than or equal to 95%2O3Is less than or equal to 0.2 percent by mass, SiO2The mass percentage content of (A) is less than or equal to 0.3 percent. The balance is inevitable other impurities.
In combination with the first aspect, the particle size of the quicklime is 0.5-2.5 cm.
In combination with the first aspect, the magnesium chloride has a purity of greater than 95%.
In a second aspect, the present application provides a method for preparing the coating slurry for a graphite crucible, which at least comprises the following steps:
crushing calcium aluminate slag, adding quicklime and uniformly mixing to obtain a mixed material;
and uniformly mixing the mixed material with magnesium chloride, adding water, and uniformly stirring to obtain the coating slurry for the graphite crucible.
In combination with the second aspect, the calcium aluminate slag is pulverized to 80 to 120 mesh.
In a third aspect, the application provides the application of the coating slurry for the graphite crucible in vanadium-aluminum alloy smelting.
The fourth aspect of the present application provides a method for reducing the content of carbon impurities in a vanadium-aluminum alloy, which at least comprises the following steps: spraying the coating slurry for the graphite crucible on the graphite crucible;
naturally drying the sprayed graphite crucible for more than 6 hours, and baking the graphite crucible for 8 to 10 hours at the temperature of 350 to 450 ℃;
and (4) using the baked graphite crucible for smelting vanadium-aluminum alloy.
The graphite crucible that this application was used is the graphite crucible body that many body combination mode assembled.
In combination with the fourth aspect, the coating slurry for the graphite crucible is sprayed on the bottom and the inner side wall of the graphite crucible, and the thickness of the coating slurry for the graphite crucible is 5-15 mm.
By limiting the thickness of the coating slurry spraying, the coating can be prevented from falling off after being dried, and the influence of the excessive thickness of the coating on the feeding amount can be avoided.
The method for reducing the content of the carbon impurities in the vanadium-aluminum alloy can greatly reduce the contact probability between the carbon graphite crucible and the alloy, can effectively isolate air and the pollution of the graphite crucible to the alloy at a high temperature of 1600 plus 1800 ℃, and reduces the content of the carbon impurities in the vanadium-aluminum alloy by 8-10 percent after the method for reducing the content of the carbon impurities in the vanadium-aluminum alloy is adopted. The method provided by the application has the advantages of simple related process and equipment, convenience and rapidness in operation, no new impurities introduced into the alloy from the used raw materials, low cost and easiness in realization of large-scale and clean production.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
The embodiment provides a coating slurry for a graphite crucible, which is composed of the following raw materials in parts by weight: calcium aluminate slag: 5 parts of quicklime: 100 portions (the mass percentage of CaO in the quicklime is 98 percent, Fe2O3Is 0.2 percent by mass, SiO20.3% by mass, 0.5cm particle size), magnesium chloride: 50 parts (96% purity) and deionized water: 150 parts;
the preparation method at least comprises the following steps: crushing calcium aluminate slag to 100-120 meshes, adding quicklime, and uniformly mixing to obtain a mixed material;
and uniformly mixing the mixed material with magnesium chloride, adding water, and uniformly stirring to obtain the coating slurry for the graphite crucible.
Example 2
The embodiment provides a coating slurry for a graphite crucible, which is composed of the following raw materials in parts by weight: calcium aluminate slag: 20 parts of quicklime: 50 portions (the weight percentage content of CaO in the quicklime is 99 percent, Fe2O3Is 0.1 percent by mass, SiO20.3% by mass, particle size of 2.5cm), magnesium chloride: 2 parts (96% purity) and deionized water: 500 parts;
the preparation method at least comprises the following steps: crushing the calcium aluminate slag to 80-100 meshes, adding quick lime, and uniformly mixing to obtain a mixed material;
and uniformly mixing the mixed material with magnesium chloride, adding water, and uniformly stirring to obtain the coating slurry for the graphite crucible.
Example 3
The embodiment provides a coating slurry for a graphite crucible, which is composed of the following raw materials in parts by weight: calcium aluminate slag: 15 parts of quicklime: 75 portions (the mass percentage of CaO in the quicklime is 98 percent, Fe2O3Is 0.2 percent by mass, SiO20.2% by mass, 1.5cm particle size), magnesium chloride: 25 parts (purity 98%) and deionized water: 325 parts of;
the preparation method at least comprises the following steps: crushing the calcium aluminate slag to 80-100 meshes, adding quick lime, and uniformly mixing to obtain a mixed material;
and (3) uniformly mixing the mixed material with magnesium chloride, adding water, and uniformly stirring to obtain the coating slurry for the graphite crucible.
Example 4
The embodiment provides a coating slurry for a graphite crucible, which is composed of the following raw materials in parts by weight: calcium aluminate slag: 12 parts of quicklime: 80 portions (the mass percentage of CaO in the quicklime is 98 percent, Fe2O3Is 0.2 percent by mass, SiO20.3% by mass, 2cm particle size), magnesium chloride: 30 parts (purity 98%) and deionized water: 400 parts of (1);
the preparation method at least comprises the following steps: crushing calcium aluminate slag to 90-110 meshes, adding quick lime, and uniformly mixing to obtain a mixed material;
and uniformly mixing the mixed material with magnesium chloride, adding water, and uniformly stirring to obtain the coating slurry for the graphite crucible.
Example 5
The embodiment provides a method for reducing the content of carbon impurities in a vanadium-aluminum alloy, which comprises the steps of spraying the coating slurry for the graphite crucible in the embodiment 1 onto the bottom and the inner side wall of the graphite crucible, wherein the spraying thickness is 15 mm;
naturally drying the sprayed graphite crucible for 6h, and baking for 8h at 450 ℃;
and (3) using the baked graphite crucible for smelting vanadium-aluminum alloy, wherein V in the obtained vanadium-aluminum alloy is as follows: 58.2%, Fe: 0.21%, Si: 0.15 percent, 0.03 percent of C, 0.04 percent of N, 0.08 percent of O and the balance of Al, and the product meets the requirement standard of high-end customized customers.
Example 6
The embodiment provides a method for reducing the content of carbon impurities in a vanadium-aluminum alloy, wherein the coating slurry for the graphite crucible in the embodiment 2 is sprayed on the bottom and the inner side wall of the graphite crucible, and the spraying thickness is 5 mm;
naturally drying the sprayed graphite crucible for 8 hours in air, and baking for 10 hours at 350 ℃;
and (3) using the baked graphite crucible for smelting vanadium-aluminum alloy, wherein V in the obtained vanadium-aluminum alloy is as follows: 58.3%, Fe: 0.18%, Si: 0.14 percent, 0.03 percent of C, 0.03 percent of N, 0.07 percent of O and the balance of Al, and the product meets the requirement standard of high-end customized customers.
Example 7
The embodiment provides a method for reducing the content of carbon impurities in a vanadium-aluminum alloy, which comprises the steps of spraying the coating slurry for the graphite crucible in the embodiment 3 onto the bottom and the inner side wall of the graphite crucible, wherein the spraying thickness is 10 mm;
naturally drying the sprayed graphite crucible for 7 hours, and baking for 9 hours at 400 ℃;
and (3) using the baked graphite crucible for smelting vanadium-aluminum alloy, wherein V in the obtained vanadium-aluminum alloy is as follows: 58.2%, Fe: 0.18%, Si: 0.15 percent, 0.03 percent of C, 0.03 percent of N, 0.06 percent of O and the balance of Al, and the product meets the requirement standard of high-end customized customers.
Example 8
The embodiment provides a method for reducing the content of carbon impurities in a vanadium-aluminum alloy, the coating slurry for the graphite crucible in the embodiment 4 is sprayed on the bottom and the inner side wall of the graphite crucible, and the spraying thickness is 13 mm;
naturally drying the sprayed graphite crucible in air for 7.5h, and baking at 380 ℃ for 9.5 h;
and (3) using the baked graphite crucible for smelting vanadium-aluminum alloy, wherein V in the obtained vanadium-aluminum alloy is as follows: 58.3%, Fe: 0.17%, Si: 0.15 percent, 0.03 percent of C, 0.04 percent of N, 0.06 percent of O and the balance of Al, and the product meets the requirement standard of high-end customized customers.
Comparative example 1
This comparative example provides the results tested during the studyThe coating slurry consists of the following raw materials in parts by weight: calcium aluminate slag: 15 parts of quicklime: 75 portions (the mass percentage of CaO in the quicklime is 98 percent, Fe2O3Is 0.2 percent of SiO20.2% by mass, 1.5cm particle size), magnesium chloride: 25 parts (purity 98%) and deionized water: 325 parts of;
the preparation method at least comprises the following steps: crushing the calcium aluminate slag to 80-100 meshes, adding quick lime, and uniformly mixing to obtain a mixed material;
and uniformly mixing the mixed material with magnesium chloride, adding water, and uniformly stirring to obtain the coating slurry for the graphite crucible.
Comparative example 2
The comparative example provides a coating slurry tested in the research process, which consists of the following raw materials in parts by weight: calcium aluminate slag: 12 parts of quicklime: 80 portions (the mass percentage of CaO in the quicklime is 98 percent, Fe2O3Is 0.2 percent by mass, SiO20.3% by mass, 2cm particle size), magnesium chloride: 30 parts (purity 98%) and deionized water: 400 parts of (1);
the preparation method at least comprises the following steps: crushing calcium aluminate slag to 90-110 meshes, adding quick lime, and uniformly mixing to obtain a mixed material;
and uniformly mixing the mixed material with magnesium chloride, adding water, and uniformly stirring to obtain the coating slurry for the graphite crucible.
Comparative example 3
The comparative example provides a method for reducing the content of carbon impurities in vanadium-aluminum alloy tested in the research process, the coating slurry for the graphite crucible in the comparative example 1 is sprayed on the bottom and the inner side wall of the graphite crucible, and the spraying thickness is 10 mm;
naturally drying the sprayed graphite crucible for 7 hours, and baking for 9 hours at 400 ℃;
and (3) using the baked graphite crucible for smelting vanadium-aluminum alloy, wherein V in the obtained vanadium-aluminum alloy is as follows: 58.2%, Fe: 0.18%, Si: 0.15 percent, 0.06 percent of C, 0.05 percent of N, 0.06 percent of O and the balance of Al.
Comparative example 4
The comparative example provides a method for reducing the content of carbon impurities in vanadium-aluminum alloy tested in the research process, the coating slurry for the graphite crucible in the comparative example 2 is sprayed on the bottom and the inner side wall of the graphite crucible, and the spraying thickness is 13 mm;
naturally drying the sprayed graphite crucible in air for 7.5h, and baking at 380 ℃ for 9.5 h;
and (3) using the baked graphite crucible for smelting vanadium-aluminum alloy, wherein V in the obtained vanadium-aluminum alloy is as follows: 58.3%, Fe: 0.17%, Si: 0.16 percent, 0.05 percent of C, 0.04 percent of N, 0.08 percent of O and the balance of Al.
Comparative example 5
The comparison example provides that the existing method is adopted to smelt vanadium-aluminum alloy, a common graphite crucible is used for smelting vanadium-aluminum alloy, and V in the obtained vanadium-aluminum alloy is as follows: 58-58.5%, Fe 0.21-0.24%, Si: 0.14-0.18 percent of C, 0.11-0.13 percent of N, 0.06-0.08 percent of O, 0.11-0.13 percent of Al in balance.
By comparing the contents of the components in the vanadium-aluminum alloys obtained in examples 5 to 8 and comparative examples 3 to 5, it can be seen that the coating slurry for the graphite crucible provided by the application can significantly reduce the content of carbon impurities in the vanadium-aluminum alloy.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (10)

1. The coating slurry for the graphite crucible is characterized by comprising the following raw materials in parts by weight: calcium aluminate slag: 5-20 parts of quicklime: 50-100 parts of magnesium chloride: 2-50 parts and deionized water: 150-500 parts.
2. The coating slurry for a graphite crucible as set forth in claim 1, wherein: the calcium aluminate furnace slag is a byproduct obtained by smelting vanadium-aluminum alloy.
3. Such as rightA coating slurry for a graphite crucible according to claim 1, wherein: the mass percentage of CaO in the quicklime is more than or equal to 95 percent, and the mass percentage of Fe in the quicklime2O3Is less than or equal to 0.2 percent by mass, SiO2The mass percentage content of (A) is less than or equal to 0.3 percent.
4. The coating slurry for a graphite crucible as set forth in claim 1, wherein: the particle size of the quicklime is 0.5-2.5 cm.
5. The coating slurry for a graphite crucible as set forth in claim 1, wherein: the purity of the magnesium chloride is more than 95%.
6. The method for preparing a coating slurry for a graphite crucible as set forth in any one of claims 1 to 5, characterized by comprising at least the steps of:
crushing the calcium aluminate slag, adding the quick lime, and uniformly mixing to obtain a mixed material;
and uniformly mixing the mixed material with the magnesium chloride, adding water, and uniformly stirring to obtain the coating slurry for the graphite crucible.
7. The method of preparing a coating slurry for a graphite crucible according to claim 6, wherein: and crushing the calcium aluminate slag to 80-120 meshes.
8. Use of the coating slip for graphite crucibles according to any one of claims 1 to 5 for smelting vanadium-aluminium alloys.
9. A method for reducing the content of carbon impurities in a vanadium-aluminum alloy is characterized by at least comprising the following steps: spraying the coating slurry for a graphite crucible as claimed in any one of claims 1 to 5 on a graphite crucible;
naturally drying the sprayed graphite crucible for more than 6 hours, and baking the graphite crucible for 8 to 10 hours at the temperature of 350 to 450 ℃;
and (4) using the baked graphite crucible for smelting vanadium-aluminum alloy.
10. The method for reducing the carbon impurity content in the vanadium-aluminum alloy according to claim 9, wherein: and spraying the coating slurry for the graphite crucible on the bottom and the inner side wall of the graphite crucible, wherein the thickness of the coating slurry for the graphite crucible is 5-15 mm.
CN202210248159.XA 2022-03-14 2022-03-14 Coating slurry for graphite crucible and preparation and application methods thereof Pending CN114702848A (en)

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CN117305985A (en) * 2023-11-29 2023-12-29 北京青禾晶元半导体科技有限责任公司 Graphite crucible, preparation method thereof and silicon carbide single crystal growth method
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