CN116120826A - Preparation method of normal-temperature self-drying high-temperature anti-corrosion nano ceramic coating - Google Patents

Preparation method of normal-temperature self-drying high-temperature anti-corrosion nano ceramic coating Download PDF

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CN116120826A
CN116120826A CN202310314567.5A CN202310314567A CN116120826A CN 116120826 A CN116120826 A CN 116120826A CN 202310314567 A CN202310314567 A CN 202310314567A CN 116120826 A CN116120826 A CN 116120826A
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陈嘉力
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Guangdong Zhongke Jingna New Material Technology Co ltd
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Abstract

The invention discloses a preparation method of a normal-temperature self-drying high-temperature anti-corrosion nano ceramic coating. Firstly, uniformly dispersing alumina fiber and carbon powder in slurry through ball milling, then, carrying out carburization treatment on ceramic powder, adding part of rare earth elements, and finally, mixing the slurry with the ceramic powder containing the rare earth elements through a stirring paddle to obtain the anti-corrosion nano ceramic coating. Compared with the traditional process, the preparation method of the normal-temperature self-drying high-temperature anti-corrosion nano ceramic coating improves the heat insulation effect of the ceramic coating, has outstanding thermal shock resistance and sintering strength, and is suitable for industrial popularization.

Description

Preparation method of normal-temperature self-drying high-temperature anti-corrosion nano ceramic coating
Technical Field
The invention relates to the technical field of nano ceramic coating, in particular to a preparation method of a normal-temperature self-drying high-temperature anti-corrosion nano ceramic coating.
Background
Along with the rapid development of modern industry and national defense construction (such as aerospace, aviation, weapons and the like) industry, the requirements on high-temperature resistant coatings of equipment are higher and higher, and paint films are required to be free from color change and falling at high temperature, and good physical and mechanical properties and corrosion resistance can be still maintained. In the field of utility boilers, the problems of contamination and slagging are particularly pronounced in recent years due to the variability of the fuel used in utility boilers. The problems of insufficient heat absorption of the water cooling wall, high smoke temperature at the outlet of the hearth, slag hanging on a convection heating surface, overtemperature of the pipe wall, excessive input of the temperature reducing water and the like are frequently encountered in the operation, so that the safe and stable operation of the power station boiler and the economical efficiency of a unit are greatly influenced.
The high temperature resistant paint is also called heat resistant paint, and is special functional paint capable of maintaining proper physical and mechanical performance at 200 deg.c and below and with paint film with no color change and no falling off and making the protected object function normally in high temperature environment. Therefore, the high-temperature resistant coating is widely applied to high-temperature places such as steel chimneys, high-temperature pipelines, high-temperature furnace shells, petroleum cracking devices, tanks, artillery and the like, delays the hot hydrogenation corrosion of metal equipment such as steel and the like at high temperature, and ensures that the equipment can be used for a long time. At present, a plurality of reports are made on the heat-resistant paint, and the heat resistance of the existing heat-resistant paint basically meets the use requirement, but has some defects. If the surface drying time of the paint film is long, the appearance of the paint film is affected due to dust and the like in the use process; poor corrosion resistance at high temperatures, and the like.
The high-temperature nano ceramic material coating has a plurality of excellent technological properties of high-temperature corrosion resistance, wear resistance, contamination resistance, slag bonding resistance and the like. The high-temperature nano ceramic coating is formed by spraying composite rare earth nano ceramic slurry on the surface of a metal or non-metal substrate, drying, solidifying and heating the composite rare earth nano ceramic slurry, has excellent high-temperature stability, corrosion resistance, hardness and non-wettability surface mechanical properties, is purple and dense with the substrate in a chemical bond form, and can comprehensively improve the surface physical and chemical properties of the substrate.
The high-temperature nano ceramic material coating has the following action mechanism:
1. the compact ceramic film isolates the contact between the matrix and the external environment, exerts the performances of oxidation resistance, high-temperature corrosion resistance, wear resistance and the like of the nano ceramic coating, is attached to the surface of the substrate, comprehensively improves the performance and the accessibility of the matrix material, and effectively prevents the oxidation, the high-temperature corrosion and the wear of the matrix material.
2. The nano ceramic coating is processed by a nano process according to a special formula, has small specific surface energy, so that molten ash particles are difficult to adhere to a heating surface, and has good contamination and slag bonding resistance.
3. The nano ceramic coating has high emissivity and high heat conductivity, can improve the blackness of the water-cooled wall after spraying, enhances the heat absorption capacity of the water-cooled wall, reduces the overall temperature of the hearth, and can operate at a relatively low temperature level by the matrix material.
At present, china has entered a rapid development period of high-tech products, but the field of paint, particularly the field of paint with special functions, still falls behind western countries, and the development of nano ceramic paint is relatively slow although the nano ceramic paint has appeared in China for many years. The problems of high cost, poor mechanical property, complicated construction process, high curing condition requirement and the like limit the application field of the ceramic coating besides a certain gap between the technical strength and foreign enterprises, and are also main reasons. The inorganic ceramic coating is healthy and environment-friendly, and particularly has good incombustibility, nontoxic gas release at high temperature and the like. Attention has been paid more and more in recent years.
Through the prior art and document retrieval, the following steps are found: patent document (CN 106977983B) discloses a normal temperature curable nanoceramic coating comprising an a-component consisting of silica sol, pigment, filler and water, and a B-component consisting of siloxane, auxiliary agent, drier and solvent. In addition, the invention also discloses a preparation method of the normal-temperature-curable nano ceramic coating, which comprises the following steps: step 1, weighing corresponding components of silica sol, pigment, filler and water, mixing, stirring the obtained mixture, grinding the uniformly stirred mixture until the fineness of the mixture is below 25 mu m, and taking the mixture as a component A; weighing corresponding components of siloxane, auxiliary agent, drier and solvent, mixing, uniformly stirring the obtained mixture, and taking the mixture as a component B; and 3, fully mixing the component A and the component B according to the proportion to generate the nano ceramic coating.
Patent document (CN 105860609A) discloses a high temperature resistant anticorrosive ceramic coating, which comprises the following raw materials in parts by weight: 10-15 parts of silica sol, 15-20 parts of aluminum dihydrogen phosphate, 5-10 parts of glass powder, 25-35 parts of ceramic micro powder, 1-5 parts of dicyclopentadienyl oxyethyl acrylate and 20-30 parts of water.
The above method optimizes the properties of the ceramic slurry by adjusting the composition of the ceramic slurry. The ceramic slurry prepared by the simple material stacking method has limited thermal shock resistance, heat insulation effect and high temperature resistance. The method aims at heat insulation and corrosion resistance of ceramic slurry. High temperature resistance. The ceramic slurry with thermal shock resistance is obtained through double improvements of the process and the components, and is suitable for large-scale industrial popularization.
Disclosure of Invention
The invention aims to provide a preparation method of a normal-temperature self-drying high-temperature anti-corrosion nano ceramic coating, which has obvious gain effect on improving the performance of the high-temperature anti-corrosion nano ceramic coating under the improvement of related processes and raw materials.
The method is based on the principle that: 1. the purpose of mixing alumina fibers in the self-drying slurry is to use the alumina fibers as a reinforcement, so that the strength of the slurry after drying is ensured; 2. the carbon powder is added to be used as a pore-forming agent in the later high-temperature sintering process, and micron-sized vacuum or semi-vacuum micropores are prepared in the ceramic coating, so that the heat insulation effect is achieved; 3. the preferential mixing of the alumina fibers into the self-drying slurry is due to the inability to sufficiently disperse the alumina fibers with simple stirring, and the energy of ball milling is much greater than that of mechanical stirring; 4. mixing carbon powder and silicon carbide together, ball milling and then mixing with self-drying slurry, wherein the silicon carbide is coated with the carbon powder, and the carbon powder is uniformly dispersed into the slurry by the silicon carbide; 5. the ceramic powder is carburized, so that the strength of the ceramic powder can be obviously increased; 6. the rare earth elements are added to modify the ceramic, so that various properties of the final ceramic coating, including strength, thermal shock and the like, are improved.
The method is characterized in that 1. The alumina ceramic fiber can be fully dispersed in slurry without agglomeration and segregation, so that the cracking of a coating caused by the difference of thermal stress in the later sintering is avoided; 2. as with alumina fiber, carbon powder is required to be uniformly distributed in slurry, and uneven distribution of pore-forming agent can lead to uneven distribution of pores in the later-stage coating, and also can cause difference of thermal stress to influence the service life of the coating; 3. after carburization treatment of the ceramic powder, the ceramic powder can be pseudo-agglomerated, which is required to be crushed in the subsequent ball milling process, so that the non-uniformity of the particle size of the powder is avoided.
The invention relates to a preparation method of a normal-temperature self-drying high-temperature anti-corrosion nano ceramic coating, which comprises the following specific implementation steps:
step S1, preparing raw materials according to mass proportion;
the raw materials are prepared according to the mass ratio: 20-45 parts of aqueous polyurethane resin, 15-35 parts of aqueous saturated polyester resin, 10-30 parts of aqueous organic silicon resin, 2-7 parts of n-butyl titanate, 2-7 parts of ethyl cellulose, 1-5 parts of alumina fiber, 25-35 parts of zirconia, 20-40 parts of silica, 15-25 parts of feldspar, 5-15 parts of boron nitride, 5-15 parts of silicon carbide, 0.4-0.8 part of cerium oxide, 0.1-0.3 part of yttrium oxide, 0.1-0.3 part of lanthanum oxide and 2-4 parts of carbon powder;
s2, preparing self-drying slurry through a ball milling process;
mixing and ball milling aqueous polyurethane resin, aqueous saturated polyester resin, aqueous organic silicon resin, n-butyl titanate and ethyl cellulose according to a configuration proportion to obtain a solvent, wherein the ball milling time is 6-10h, the ball milling medium is zirconium balls, and the ball milling rotating speed is 200-400rpm;
mixing and ball milling alumina fiber, silicon carbide and 1-2 parts of carbon powder to obtain mixed ceramic powder, wherein the ball milling time is 2-3h, and the ball milling rotating speed is 100-200rpm to obtain mixed powder I containing carbon powder;
carrying out three ball milling treatments on the mixed powder containing carbon powder and a solvent, wherein the ball milling time is 1-2h, and the ball milling rotating speed is 100-200rpm to obtain self-drying slurry;
step S3, obtaining ceramic oxide containing a carburized layer through carburization treatment;
mixing and ball milling zirconium oxide, silicon dioxide, feldspar and 1-2 parts of carbon powder to obtain mixed ceramic powder, wherein the ball milling time is 3-5h, and the ball milling rotating speed is 200-400rpm to obtain mixed powder II containing carbon powder;
carburizing the mixed ceramic powder, wherein the carburizing temperature is 1000-1400 ℃, the treatment time is 2-4h, the treatment atmosphere is vacuum, and the vacuum degree is 0.1-0.5pa, and finally obtaining ceramic oxide containing a carburized layer;
s4, obtaining a mixture of ceramic powder through ball milling treatment;
mixing and ball milling ceramic oxide containing carburized layer, cerium oxide, yttrium oxide and lanthanum oxide for 1-3h at 200-400rpm to obtain ceramic powder mixture;
s5, obtaining ceramic paint through stirring and ultrasonic technology;
stirring the mixture of the ceramic powder and the self-drying slurry, and performing ultrasonic dispersion, wherein the stirring speed is 100-200rpm, and the stirring time is 30-60min to obtain the ceramic coating.
The beneficial effects are that:
(1) The invention designs a preparation method of a normal-temperature self-drying high-temperature anti-corrosion nano ceramic coating, which utilizes alumina fibers to form 'connection' in a material, ensures the strength of the material before and after sintering, and improves the thermal shock resistance of the material;
(2) The invention designs a preparation method of a normal-temperature self-drying high-temperature anti-corrosion nano ceramic coating, which uses carbon powder as a pore-forming agent to form vacuum or semi-vacuum micron-sized holes in a ceramic coating, and has obvious improvement effect on the heat insulation effect of the coating;
(3) The invention designs a preparation method of a normal-temperature self-drying high-temperature anti-corrosion nano ceramic coating, which is characterized in that the obtained ceramic powder has good surface strength and anti-corrosion capability by carburizing the ceramic powder;
(4) The invention designs a preparation method of a normal-temperature self-drying high-temperature anti-corrosion nano ceramic coating, which is characterized in that rare earth elements are added into slurry to modify ceramic powder, so that the sintering activity and the surface hardness of ceramic are improved well.
Drawings
FIG. 1 is a preparation flow chart of a preparation method of a normal temperature self-drying high temperature anti-corrosive nano ceramic coating.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
The embodiment of the invention provides a preparation method of a normal-temperature self-drying high-temperature anti-corrosion nano ceramic coating, which mainly comprises the following steps:
step S1, preparing raw materials according to mass proportion;
specifically, the raw materials are prepared according to the mass ratio: 20-45 parts of aqueous polyurethane resin, 15-35 parts of aqueous saturated polyester resin, 10-30 parts of aqueous organic silicon resin, 2-7 parts of n-butyl titanate, 2-7 parts of ethyl cellulose, 1-5 parts of alumina fiber, 25-35 parts of zirconia, 20-40 parts of silica, 15-25 parts of feldspar, 5-15 parts of boron nitride, 5-15 parts of silicon carbide, 0.4-0.8 part of cerium oxide, 0.1-0.3 part of yttrium oxide, 0.1-0.3 part of lanthanum oxide and 2-4 parts of carbon powder;
s2, preparing self-drying slurry through a ball milling process;
mixing and ball milling aqueous polyurethane resin, aqueous saturated polyester resin, aqueous organic silicon resin, n-butyl titanate and ethyl cellulose according to a configuration proportion to obtain a solvent;
mixing and ball milling alumina fiber, silicon carbide and 1-2 parts of carbon powder to obtain mixed ceramic powder;
carrying out ball milling on the mixed powder containing carbon powder and a solvent for three times to obtain self-drying slurry;
step S3, obtaining ceramic oxide containing a carburized layer through carburization treatment;
mixing and ball milling zirconium oxide, silicon dioxide, feldspar and 1-2 parts of carbon powder to obtain mixed ceramic powder;
carburizing the mixed ceramic powder to obtain ceramic oxide containing a carburized layer;
s4, obtaining a mixture of ceramic powder through ball milling treatment;
mixing and ball milling ceramic oxide containing carburized layer with cerium oxide, yttrium oxide and lanthanum oxide to obtain a mixture of ceramic powder;
and S5, obtaining the ceramic coating through stirring and ultrasonic processes.
Stirring the mixture of the ceramic powder and the self-drying slurry, and performing ultrasonic dispersion to obtain a ceramic coating;
as an example, the following description of the preparation method of the normal-temperature self-drying high-temperature anti-corrosion nano ceramic coating is given by the following examples of example 1, example 2, example 3 and examples 1-8.
Example 1:
step S1, preparing raw materials according to mass proportion;
the raw materials are prepared according to the mass ratio: 20 parts of aqueous polyurethane resin, 15 parts of aqueous saturated polyester resin, 10 parts of aqueous organic silicon resin, 2 parts of n-butyl titanate, 2 parts of ethyl cellulose, 1 part of alumina fiber, 25 parts of zirconia, 20 parts of silicon dioxide, 155 parts of feldspar, 5 parts of boron nitride, 5 parts of silicon carbide, 0.4 part of cerium oxide, 0.1 part of yttrium oxide, 0.1 part of lanthanum oxide and 2 parts of carbon powder;
s2, preparing self-drying slurry through a ball milling process;
mixing and ball milling aqueous polyurethane resin, aqueous saturated polyester resin, aqueous organic silicon resin, n-butyl titanate and ethyl cellulose according to a configuration proportion to obtain a solvent, wherein the ball milling time is 6 hours, the ball milling medium is zirconium balls, and the ball milling rotating speed is 200rpm;
mixing and ball-milling alumina fiber, silicon carbide and 1 part of carbon powder to obtain mixed ceramic powder, wherein the ball-milling time is 2h, and the ball-milling rotating speed is 100rpm to obtain mixed powder I containing the carbon powder;
carrying out three ball milling treatments on the mixed powder containing carbon powder and a solvent, wherein the ball milling time is 1-2h, and the ball milling rotating speed is 100rpm to obtain self-drying slurry;
step S3, obtaining ceramic oxide containing a carburized layer through carburization treatment;
mixing zirconia, silica, feldspar and 1 part of carbon powder, ball milling to obtain mixed ceramic powder, wherein the ball milling time is 3h, and the ball milling rotating speed is 200rpm to obtain mixed powder II containing carbon powder;
carburizing the mixed ceramic powder, wherein the carburizing temperature is 1000 ℃, the treatment time is 2 hours, the treatment atmosphere is vacuum, and the vacuum degree is 0.1pa, and finally obtaining ceramic oxide containing a carburized layer;
s4, obtaining a mixture of ceramic powder through ball milling treatment;
mixing and ball milling ceramic oxide containing carburized layer, cerium oxide, yttrium oxide and lanthanum oxide for 1h at 200rpm to obtain a mixture of ceramic powder;
s5, obtaining ceramic paint through stirring and ultrasonic technology;
and stirring the mixture of the ceramic powder and the self-drying slurry, and performing ultrasonic dispersion, wherein the stirring speed is 100rpm, and the stirring time is 30min, so as to obtain the ceramic coating.
Example 2:
step S1, preparing raw materials according to mass proportion;
the raw materials are prepared according to the mass ratio: 45 parts of aqueous polyurethane resin, 35 parts of aqueous saturated polyester resin, 30 parts of aqueous organic silicon resin, 7 parts of n-butyl titanate, 7 parts of ethyl cellulose, 5 parts of alumina fiber, 35 parts of zirconia, 40 parts of silicon dioxide, 25 parts of feldspar, 15 parts of boron nitride, 15 parts of silicon carbide, 0.8 part of cerium oxide, 0.3 part of yttrium oxide, 0.3 part of lanthanum oxide and 4 parts of carbon powder;
s2, preparing self-drying slurry through a ball milling process;
mixing and ball milling aqueous polyurethane resin, aqueous saturated polyester resin, aqueous organic silicon resin, n-butyl titanate and ethyl cellulose according to a configuration proportion to obtain a solvent, wherein the ball milling time is 10 hours, the ball milling medium is zirconium balls, and the ball milling rotating speed is 400rpm;
mixing and ball-milling alumina fiber, silicon carbide and 2 parts of carbon powder to obtain mixed ceramic powder, wherein the ball-milling time is 3h, and the ball-milling rotating speed is 200rpm to obtain mixed powder I containing the carbon powder;
carrying out three ball milling treatments on the mixed powder containing carbon powder and a solvent, wherein the ball milling time is 2 hours, and the ball milling rotating speed is 200rpm to obtain self-drying slurry;
step S3, obtaining ceramic oxide containing a carburized layer through carburization treatment;
mixing and ball-milling zirconium oxide, silicon dioxide, feldspar and 2 parts of carbon powder to obtain mixed ceramic powder, wherein the ball-milling time is 5 hours, and the ball-milling rotating speed is 400rpm to obtain mixed powder II containing the carbon powder;
carburizing the mixed ceramic powder, wherein the carburizing temperature is 1400 ℃, the treatment time is 4 hours, the treatment atmosphere is vacuum, and the vacuum degree is 0.5pa, and finally obtaining ceramic oxide containing a carburized layer;
s4, obtaining a mixture of ceramic powder through ball milling treatment;
mixing and ball milling ceramic oxide containing carburized layer, cerium oxide, yttrium oxide and lanthanum oxide for 3h at 400rpm to obtain ceramic powder mixture;
s5, obtaining ceramic paint through stirring and ultrasonic technology;
and stirring the mixture of the ceramic powder and the self-drying slurry, and performing ultrasonic dispersion, wherein the stirring speed is 200rpm, and the stirring time is 60min to obtain the ceramic coating.
Example 3:
step S1, preparing raw materials according to mass proportion;
the raw materials are prepared according to the mass ratio: 30 parts of aqueous polyurethane resin, 25 parts of aqueous saturated polyester resin, 20 parts of aqueous organic silicon resin, 5 parts of n-butyl titanate, 5 parts of ethyl cellulose, 3 parts of alumina fiber, 30 parts of zirconia, 30 parts of silicon dioxide, 20 parts of feldspar, 10 parts of boron nitride, 10 parts of silicon carbide, 0.6 part of cerium oxide, 0.2 part of yttrium oxide, 0.2 part of lanthanum oxide and 3 parts of carbon powder;
s2, preparing self-drying slurry through a ball milling process;
mixing and ball milling aqueous polyurethane resin, aqueous saturated polyester resin, aqueous organic silicon resin, n-butyl titanate and ethyl cellulose according to a configuration proportion to obtain a solvent, wherein the ball milling time is 8 hours, the ball milling medium is zirconium balls, and the ball milling rotating speed is 300rpm;
mixing and ball-milling alumina fiber, silicon carbide and 2 parts of carbon powder to obtain mixed ceramic powder, wherein the ball-milling time is 3h, and the ball-milling rotating speed is 150rpm to obtain mixed powder I containing the carbon powder;
carrying out three ball milling treatments on the mixed powder containing carbon powder and a solvent, wherein the ball milling time is 2 hours, and the ball milling rotating speed is 150rpm to obtain self-drying slurry;
step S3, obtaining ceramic oxide containing a carburized layer through carburization treatment;
mixing zirconia, silica, feldspar and 1 part of carbon powder, ball milling to obtain mixed ceramic powder, wherein the ball milling time is 4 hours, and the ball milling rotating speed is 300rpm to obtain mixed powder II containing the carbon powder;
carburizing the mixed ceramic powder, wherein the carburizing temperature is 1200 ℃, the treatment time is 3 hours, the treatment atmosphere is vacuum, and the vacuum degree is 0.3pa, and finally obtaining ceramic oxide containing a carburized layer;
s4, obtaining a mixture of ceramic powder through ball milling treatment;
mixing and ball milling ceramic oxide containing carburized layer, cerium oxide, yttrium oxide and lanthanum oxide for 2h at 300rpm to obtain ceramic powder mixture;
s5, obtaining ceramic paint through stirring and ultrasonic technology;
and stirring the mixture of the ceramic powder and the self-drying slurry, and performing ultrasonic dispersion, wherein the stirring speed is 150rpm, and the stirring time is 40min to obtain the ceramic coating.
Comparative example 1:
step S1, preparing raw materials according to mass proportion;
the raw materials are prepared according to the mass ratio: 30 parts of aqueous polyurethane resin, 25 parts of aqueous saturated polyester resin, 20 parts of aqueous organic silicon resin, 5 parts of n-butyl titanate, 5 parts of ethyl cellulose, 30 parts of zirconium oxide, 30 parts of silicon dioxide, 20 parts of feldspar, 10 parts of boron nitride, 10 parts of silicon carbide, 0.6 part of cerium oxide, 0.2 part of yttrium oxide, 0.2 part of lanthanum oxide and 3 parts of carbon powder;
s2, preparing self-drying slurry through a ball milling process;
mixing and ball milling aqueous polyurethane resin, aqueous saturated polyester resin, aqueous organic silicon resin, n-butyl titanate and ethyl cellulose according to a configuration proportion to obtain a solvent, wherein the ball milling time is 8 hours, the ball milling medium is zirconium balls, and the ball milling rotating speed is 300rpm;
mixing and ball milling silicon carbide and 2 parts of carbon powder to obtain mixed ceramic powder, wherein the ball milling time is 3h, and the ball milling rotating speed is 150rpm to obtain mixed powder I containing carbon powder;
carrying out three ball milling treatments on the mixed powder containing carbon powder and a solvent, wherein the ball milling time is 2 hours, and the ball milling rotating speed is 150rpm to obtain self-drying slurry;
step S3, obtaining ceramic oxide containing a carburized layer through carburization treatment;
mixing zirconia, silica, feldspar and 1 part of carbon powder, ball milling to obtain mixed ceramic powder, wherein the ball milling time is 4 hours, and the ball milling rotating speed is 300rpm to obtain mixed powder II containing the carbon powder;
carburizing the mixed ceramic powder, wherein the carburizing temperature is 1200 ℃, the treatment time is 3 hours, the treatment atmosphere is vacuum, and the vacuum degree is 0.3pa, and finally obtaining ceramic oxide containing a carburized layer;
s4, obtaining a mixture of ceramic powder through ball milling treatment;
mixing and ball milling ceramic oxide containing carburized layer, cerium oxide, yttrium oxide and lanthanum oxide for 2h at 300rpm to obtain ceramic powder mixture;
s5, obtaining ceramic paint through stirring and ultrasonic technology;
and stirring the mixture of the ceramic powder and the self-drying slurry, and performing ultrasonic dispersion, wherein the stirring speed is 150rpm, and the stirring time is 40min to obtain the ceramic coating.
Comparative example 2:
step S1, preparing raw materials according to mass proportion;
the raw materials are prepared according to the mass ratio: 30 parts of aqueous polyurethane resin, 25 parts of aqueous saturated polyester resin, 20 parts of aqueous organic silicon resin, 5 parts of n-butyl titanate, 5 parts of ethyl cellulose, 3 parts of alumina fiber, 30 parts of zirconia, 30 parts of silicon dioxide, 20 parts of feldspar, 10 parts of boron nitride and 10 parts of silicon carbide;
s2, preparing self-drying slurry through a ball milling process;
mixing and ball milling aqueous polyurethane resin, aqueous saturated polyester resin, aqueous organic silicon resin, n-butyl titanate and ethyl cellulose according to a configuration proportion to obtain a solvent, wherein the ball milling time is 8 hours, the ball milling medium is zirconium balls, and the ball milling rotating speed is 300rpm;
mixing and ball-milling alumina fiber, silicon carbide and 2 parts of carbon powder to obtain mixed ceramic powder, wherein the ball-milling time is 3h, and the ball-milling rotating speed is 150rpm to obtain mixed powder I containing the carbon powder;
carrying out three ball milling treatments on the mixed powder containing carbon powder and a solvent, wherein the ball milling time is 2 hours, and the ball milling rotating speed is 150rpm to obtain self-drying slurry;
step S3, obtaining ceramic oxide containing a carburized layer through carburization treatment;
mixing zirconia, silica, feldspar and 1 part of carbon powder, ball milling to obtain mixed ceramic powder, wherein the ball milling time is 4 hours, and the ball milling rotating speed is 300rpm to obtain mixed powder II containing the carbon powder;
carburizing the mixed ceramic powder, wherein the carburizing temperature is 1200 ℃, the treatment time is 3 hours, the treatment atmosphere is vacuum, and the vacuum degree is 0.3pa, and finally obtaining ceramic oxide containing a carburized layer;
s4, obtaining a mixture of ceramic powder through ball milling treatment;
ball milling is carried out on the ceramic oxide containing the carburized layer for 2 hours at the ball milling rotating speed of 300rpm to obtain a mixture of ceramic powder;
s5, obtaining ceramic paint through stirring and ultrasonic technology;
and stirring the mixture of the ceramic powder and the self-drying slurry, and performing ultrasonic dispersion, wherein the stirring speed is 150rpm, and the stirring time is 40min to obtain the ceramic coating.
Comparative example 3:
step S1, preparing raw materials according to mass proportion;
the raw materials are prepared according to the mass ratio: 30 parts of aqueous polyurethane resin, 25 parts of aqueous saturated polyester resin, 20 parts of aqueous organic silicon resin, 5 parts of n-butyl titanate, 5 parts of ethyl cellulose, 3 parts of alumina fiber, 30 parts of zirconia, 30 parts of silicon dioxide, 20 parts of feldspar, 10 parts of boron nitride, 10 parts of silicon carbide, 0.6 part of cerium oxide, 0.2 part of yttrium oxide, 0.2 part of lanthanum oxide and 2 parts of carbon powder;
s2, preparing self-drying slurry through a ball milling process;
mixing and ball milling aqueous polyurethane resin, aqueous saturated polyester resin, aqueous organic silicon resin, n-butyl titanate and ethyl cellulose according to a configuration proportion to obtain a solvent, wherein the ball milling time is 8 hours, the ball milling medium is zirconium balls, and the ball milling rotating speed is 300rpm;
mixing and ball-milling alumina fiber, silicon carbide and 2 parts of carbon powder to obtain mixed ceramic powder, wherein the ball-milling time is 3h, and the ball-milling rotating speed is 150rpm to obtain mixed powder I containing the carbon powder;
carrying out three ball milling treatments on the mixed powder containing carbon powder and a solvent, wherein the ball milling time is 2 hours, and the ball milling rotating speed is 150rpm to obtain self-drying slurry;
step S3, obtaining a mixture of ceramic powder through ball milling treatment;
mixing zirconia, silica, feldspar, cerium oxide, yttrium oxide and lanthanum oxide, performing ball milling for 2 hours at a ball milling rotating speed of 300rpm to obtain a mixture of ceramic powder;
s4, obtaining ceramic paint through stirring and ultrasonic technology;
and stirring the mixture of the ceramic powder and the self-drying slurry, and performing ultrasonic dispersion, wherein the stirring speed is 150rpm, and the stirring time is 40min to obtain the ceramic coating.
Comparative example 4:
step S1, preparing raw materials according to mass proportion;
the raw materials are prepared according to the mass ratio: 30 parts of aqueous polyurethane resin, 25 parts of aqueous saturated polyester resin, 20 parts of aqueous organic silicon resin, 5 parts of n-butyl titanate, 5 parts of ethyl cellulose, 3 parts of alumina fiber, 30 parts of zirconia, 30 parts of silicon dioxide, 20 parts of feldspar, 10 parts of boron nitride, 10 parts of silicon carbide, 0.6 part of cerium oxide, 0.2 part of yttrium oxide, 0.2 part of lanthanum oxide and 10 parts of carbon powder;
s2, preparing self-drying slurry through a ball milling process;
mixing and ball milling aqueous polyurethane resin, aqueous saturated polyester resin, aqueous organic silicon resin, n-butyl titanate and ethyl cellulose according to a configuration proportion to obtain a solvent, wherein the ball milling time is 8 hours, the ball milling medium is zirconium balls, and the ball milling rotating speed is 300rpm;
mixing and ball-milling alumina fiber, silicon carbide and 9 parts of carbon powder to obtain mixed ceramic powder, wherein the ball-milling time is 3h, and the ball-milling rotating speed is 150rpm to obtain mixed powder I containing carbon powder;
carrying out three ball milling treatments on the mixed powder containing carbon powder and a solvent, wherein the ball milling time is 2 hours, and the ball milling rotating speed is 150rpm to obtain self-drying slurry;
step S3, obtaining ceramic oxide containing a carburized layer through carburization treatment;
mixing zirconia, silica, feldspar and 1 part of carbon powder, ball milling to obtain mixed ceramic powder, wherein the ball milling time is 4 hours, and the ball milling rotating speed is 300rpm to obtain mixed powder II containing the carbon powder;
carburizing the mixed ceramic powder, wherein the carburizing temperature is 1200 ℃, the treatment time is 3 hours, the treatment atmosphere is vacuum, and the vacuum degree is 0.3pa, and finally obtaining ceramic oxide containing a carburized layer;
s4, obtaining a mixture of ceramic powder through ball milling treatment;
mixing and ball milling ceramic oxide containing carburized layer, cerium oxide, yttrium oxide and lanthanum oxide for 2h at 300rpm to obtain ceramic powder mixture;
s5, obtaining ceramic paint through stirring and ultrasonic technology;
and stirring the mixture of the ceramic powder and the self-drying slurry, and performing ultrasonic dispersion, wherein the stirring speed is 150rpm, and the stirring time is 40min to obtain the ceramic coating.
Comparative example 5:
step S1, preparing raw materials according to mass proportion;
the raw materials are prepared according to the mass ratio: 30 parts of aqueous polyurethane resin, 25 parts of aqueous saturated polyester resin, 20 parts of aqueous organic silicon resin, 5 parts of n-butyl titanate, 5 parts of ethyl cellulose, 3 parts of alumina fiber, 30 parts of zirconia, 30 parts of silicon dioxide, 20 parts of feldspar, 10 parts of boron nitride, 0.6 part of cerium oxide, 0.2 part of yttrium oxide, 0.2 part of lanthanum oxide and 3 parts of carbon powder;
s2, preparing self-drying slurry through a ball milling process;
mixing and ball milling aqueous polyurethane resin, aqueous saturated polyester resin, aqueous organic silicon resin, n-butyl titanate and ethyl cellulose according to a configuration proportion to obtain a solvent, wherein the ball milling time is 8 hours, the ball milling medium is zirconium balls, and the ball milling rotating speed is 300rpm;
mixing and ball milling alumina fiber and 2 parts of carbon powder to obtain mixed ceramic powder, wherein the ball milling time is 3h, and the ball milling rotating speed is 150rpm to obtain mixed powder I containing carbon powder;
carrying out three ball milling treatments on the mixed powder containing carbon powder and a solvent, wherein the ball milling time is 2 hours, and the ball milling rotating speed is 150rpm to obtain self-drying slurry;
step S3, obtaining ceramic oxide containing a carburized layer through carburization treatment;
mixing zirconia, silica, feldspar and 1 part of carbon powder, ball milling to obtain mixed ceramic powder, wherein the ball milling time is 4 hours, and the ball milling rotating speed is 300rpm to obtain mixed powder II containing the carbon powder;
carburizing the mixed ceramic powder, wherein the carburizing temperature is 1200 ℃, the treatment time is 3 hours, the treatment atmosphere is vacuum, and the vacuum degree is 0.3pa, and finally obtaining ceramic oxide containing a carburized layer;
s4, obtaining a mixture of ceramic powder through ball milling treatment;
mixing and ball milling ceramic oxide containing carburized layer, cerium oxide, yttrium oxide and lanthanum oxide for 2h at 300rpm to obtain ceramic powder mixture;
s5, obtaining ceramic paint through stirring and ultrasonic technology;
and stirring the mixture of the ceramic powder and the self-drying slurry, and performing ultrasonic dispersion, wherein the stirring speed is 150rpm, and the stirring time is 40min to obtain the ceramic coating.
Comparative example 6:
step S1, preparing raw materials according to mass proportion;
the raw materials are prepared according to the mass ratio: 30 parts of aqueous polyurethane resin, 25 parts of aqueous saturated polyester resin, 20 parts of aqueous organic silicon resin, 5 parts of n-butyl titanate, 5 parts of ethyl cellulose, 3 parts of alumina fiber, 30 parts of zirconia, 30 parts of silicon dioxide, 20 parts of feldspar, 10 parts of boron nitride, 10 parts of silicon carbide, 0.6 part of cerium oxide, 0.2 part of yttrium oxide, 0.2 part of lanthanum oxide and 3 parts of carbon powder;
s2, preparing self-drying slurry through a ball milling process;
mixing and ball milling aqueous polyurethane resin, aqueous saturated polyester resin, aqueous organic silicon resin, n-butyl titanate and ethyl cellulose according to a configuration proportion to obtain a solvent, wherein the ball milling time is 8 hours, the ball milling medium is zirconium balls, and the ball milling rotating speed is 300rpm;
mixing and ball-milling alumina fiber, silicon carbide and 2 parts of carbon powder to obtain mixed ceramic powder, wherein the ball-milling time is 3h, and the ball-milling rotating speed is 150rpm to obtain mixed powder I containing the carbon powder;
carrying out three ball milling treatments on the mixed powder containing carbon powder and a solvent, wherein the ball milling time is 2 hours, and the ball milling rotating speed is 150rpm to obtain self-drying slurry;
step S3, obtaining ceramic oxide containing a carburized layer through carburization treatment;
mixing zirconia, silica, feldspar and 1 part of carbon powder, ball milling to obtain mixed ceramic powder, wherein the ball milling time is 4 hours, and the ball milling rotating speed is 300rpm to obtain mixed powder II containing the carbon powder;
carburizing the mixed ceramic powder, wherein the carburizing temperature is 1200 ℃, the treatment time is 3 hours, the treatment atmosphere is vacuum, and the vacuum degree is 0.3pa, and finally obtaining ceramic oxide containing a carburized layer;
s4, obtaining a mixture of ceramic powder through ball milling treatment;
mixing and ball milling ceramic oxide containing carburized layer, cerium oxide, yttrium oxide and lanthanum oxide for 0.5h at 50rpm to obtain ceramic powder mixture;
s5, obtaining ceramic paint through stirring and ultrasonic technology;
and stirring the mixture of the ceramic powder and the self-drying slurry, and performing ultrasonic dispersion, wherein the stirring speed is 150rpm, and the stirring time is 40min to obtain the ceramic coating.
Comparative example 7:
step S1, preparing raw materials according to mass proportion;
the raw materials are prepared according to the mass ratio: 30 parts of aqueous polyurethane resin, 25 parts of aqueous saturated polyester resin, 20 parts of aqueous organic silicon resin, 5 parts of n-butyl titanate, 3 parts of alumina fiber, 30 parts of zirconia, 30 parts of silica, 20 parts of feldspar, 10 parts of boron nitride, 10 parts of silicon carbide, 0.6 part of cerium oxide, 0.2 part of yttrium oxide, 0.2 part of lanthanum oxide and 3 parts of carbon powder;
s2, preparing self-drying slurry through a ball milling process;
mixing and ball milling aqueous polyurethane resin, aqueous saturated polyester resin, aqueous organic silicon resin and n-butyl titanate according to a configuration proportion to obtain a solvent, wherein the ball milling time is 8 hours, the ball milling medium is zirconium balls, and the ball milling rotating speed is 300rpm;
mixing and ball-milling alumina fiber, silicon carbide and 2 parts of carbon powder to obtain mixed ceramic powder, wherein the ball-milling time is 3h, and the ball-milling rotating speed is 150rpm to obtain mixed powder I containing the carbon powder;
carrying out three ball milling treatments on the mixed powder containing carbon powder and a solvent, wherein the ball milling time is 2 hours, and the ball milling rotating speed is 150rpm to obtain self-drying slurry;
step S3, obtaining ceramic oxide containing a carburized layer through carburization treatment;
mixing zirconia, silica, feldspar and 1 part of carbon powder, ball milling to obtain mixed ceramic powder, wherein the ball milling time is 4 hours, and the ball milling rotating speed is 300rpm to obtain mixed powder II containing the carbon powder;
carburizing the mixed ceramic powder, wherein the carburizing temperature is 1200 ℃, the treatment time is 3 hours, the treatment atmosphere is vacuum, and the vacuum degree is 0.3pa, and finally obtaining ceramic oxide containing a carburized layer;
s4, obtaining a mixture of ceramic powder through ball milling treatment;
mixing and ball milling ceramic oxide containing carburized layer, cerium oxide, yttrium oxide and lanthanum oxide for 2h at 300rpm to obtain ceramic powder mixture;
s5, obtaining ceramic paint through stirring and ultrasonic technology;
and stirring the mixture of the ceramic powder and the self-drying slurry, and performing ultrasonic dispersion, wherein the stirring speed is 150rpm, and the stirring time is 40min to obtain the ceramic coating.
Comparative example 8:
step S1, preparing raw materials according to mass proportion;
the raw materials are prepared according to the mass ratio: 30 parts of aqueous polyurethane resin, 25 parts of aqueous saturated polyester resin, 20 parts of aqueous organic silicon resin, 5 parts of n-butyl titanate, 5 parts of ethyl cellulose, 3 parts of alumina fiber, 30 parts of zirconia, 30 parts of silicon dioxide, 20 parts of feldspar, 10 parts of boron nitride, 10 parts of silicon carbide, 0.6 part of cerium oxide, 0.2 part of yttrium oxide, 0.2 part of lanthanum oxide and 3 parts of carbon powder;
s2, preparing self-drying slurry through a ball milling process;
mixing and ball milling aqueous polyurethane resin, aqueous saturated polyester resin, aqueous organic silicon resin, n-butyl titanate and ethyl cellulose according to a configuration proportion to obtain a solvent, wherein the ball milling time is 8 hours, the ball milling medium is zirconium balls, and the ball milling rotating speed is 300rpm;
mixing and ball milling alumina fiber and silicon carbide to obtain mixed ceramic powder, wherein the ball milling time is 3h, and the ball milling rotating speed is 150rpm to obtain mixed powder I containing carbon powder;
carrying out three ball milling treatments on the mixed powder containing carbon powder and a solvent, wherein the ball milling time is 2 hours, and the ball milling rotating speed is 150rpm to obtain self-drying slurry;
step S3, obtaining ceramic oxide containing a carburized layer through carburization treatment;
mixing zirconia, silica, feldspar and 1 part of carbon powder, ball milling to obtain mixed ceramic powder, wherein the ball milling time is 4 hours, and the ball milling rotating speed is 300rpm to obtain mixed powder II containing the carbon powder;
carburizing the mixed ceramic powder, wherein the carburizing temperature is 1200 ℃, the treatment time is 3 hours, the treatment atmosphere is vacuum, and the vacuum degree is 0.3pa, and finally obtaining ceramic oxide containing a carburized layer;
s4, obtaining a mixture of ceramic powder through ball milling treatment;
mixing and ball milling ceramic oxide containing carburized layer, cerium oxide, yttrium oxide and lanthanum oxide for 2h at 300rpm to obtain ceramic powder mixture;
s5, obtaining ceramic paint through stirring and ultrasonic technology;
and stirring and ultrasonically dispersing 2 parts of a mixture of carbon powder and ceramic powder with the self-drying slurry, wherein the stirring speed is 150rpm, and the stirring time is 40min to obtain the ceramic coating.
Table 1:
Figure BDA0004149831540000191
as can be seen from the data in Table 1, after the rare earth is used for improving the ceramic powder, the wear resistance of the ceramic coating is obviously improved, in addition, the addition of alumina fiber in the coating has obvious enhancement effect on the adhesive force and wear resistance of the material, and the independent stirring of carbon powder also has adverse effect on the performance of the coating due to uneven distribution caused by lighter mass of the carbon powder.

Claims (9)

1. The preparation method of the normal-temperature self-drying high-temperature anti-corrosion nano ceramic coating is characterized by comprising the following steps of:
preparing raw materials according to mass proportion;
preparing self-drying slurry by a ball milling process;
obtaining ceramic oxide containing a carburized layer through carburization treatment;
obtaining a mixture of ceramic powder through ball milling treatment;
the ceramic coating is obtained through stirring and ultrasonic processes.
2. The method for preparing the normal-temperature self-drying high-temperature anti-corrosion nano ceramic coating according to claim 1, which is characterized in that,
the step of preparing raw materials according to the mass ratio comprises the following steps:
the raw materials are prepared according to the mass ratio: 20-45 parts of aqueous polyurethane resin, 15-35 parts of aqueous saturated polyester resin, 10-30 parts of aqueous organic silicon resin, 2-7 parts of n-butyl titanate, 2-7 parts of ethyl cellulose, 1-5 parts of alumina fiber, 25-35 parts of zirconia, 20-40 parts of silica, 15-25 parts of feldspar, 5-15 parts of boron nitride, 5-15 parts of silicon carbide, 0.4-0.8 part of cerium oxide, 0.1-0.3 part of yttrium oxide, 0.1-0.3 part of lanthanum oxide and 2-4 parts of carbon powder;
wherein, the diameter of the alumina fiber is 1-5um, the diameter is 30-70um, the zirconia is 300 meshes, the silica is 200 meshes, the feldspar is 300 meshes, the boron nitride is 300 meshes, and the silicon carbide is 300 meshes.
The step of preparing self-drying slurry by a ball milling process comprises the following steps:
mixing and ball milling aqueous polyurethane resin, aqueous saturated polyester resin, aqueous organic silicon resin, n-butyl titanate and ethyl cellulose according to a configuration proportion to obtain a solvent;
mixing and ball milling alumina fiber, silicon carbide and 1-2 parts of carbon powder to obtain mixed ceramic powder;
carrying out ball milling on the mixed powder containing carbon powder and a solvent for three times to obtain self-drying slurry;
the step of obtaining the ceramic oxide containing the carburized layer by carburizing treatment comprises the following steps:
mixing and ball milling zirconium oxide, silicon dioxide, feldspar and 1-2 parts of carbon powder to obtain mixed ceramic powder;
carburizing the mixed ceramic powder to obtain ceramic oxide containing a carburized layer;
the step of obtaining the mixture of ceramic powder through ball milling treatment comprises the following steps:
mixing and ball milling ceramic oxide containing carburized layer with cerium oxide, yttrium oxide and lanthanum oxide to obtain a mixture of ceramic powder;
the step of obtaining the ceramic coating through stirring and ultrasonic technology comprises the following steps:
and stirring the mixture of the ceramic powder and the self-drying slurry, and performing ultrasonic dispersion to obtain the ceramic coating.
3. The method for preparing the normal-temperature self-drying high-temperature anti-corrosion nano ceramic coating according to claim 2, which is characterized in that,
the step of carrying out mixing ball milling treatment on the aqueous polyurethane resin, the aqueous saturated polyester resin, the aqueous organic silicon resin, the n-butyl titanate and the ethyl cellulose according to the configuration proportion to obtain a solvent comprises the following steps:
mixing and ball milling aqueous polyurethane resin, aqueous saturated polyester resin, aqueous organic silicon resin, n-butyl titanate and ethyl cellulose according to a configuration proportion to obtain a solvent, wherein the ball milling time is 6-10h, the ball milling medium is zirconium balls, and the ball milling rotating speed is 200-400rpm.
4. The method for preparing the normal-temperature self-drying high-temperature anti-corrosion nano ceramic coating according to claim 2, which is characterized in that,
the step of carrying out mixed ball milling on alumina fiber, silicon carbide and 1-2 parts of carbon powder to obtain mixed ceramic powder comprises the following steps:
mixing and ball milling alumina fiber, silicon carbide and 1-2 parts of carbon powder to obtain mixed ceramic powder, wherein the ball milling time is 2-3h, and the ball milling rotating speed is 100-200rpm to obtain mixed powder I containing carbon powder.
5. The method for preparing the normal-temperature self-drying high-temperature anti-corrosion nano ceramic coating according to claim 2, which is characterized in that,
the step of ball milling the mixed powder containing carbon powder and the solvent for three times to obtain self-drying slurry comprises the following steps:
and carrying out three ball milling treatments on the mixed powder containing carbon powder and the solvent, wherein the ball milling time is 1-2h, and the ball milling rotating speed is 100-200rpm, so as to obtain self-drying slurry.
6. The method for preparing the normal-temperature self-drying high-temperature anti-corrosion nano ceramic coating according to claim 2, which is characterized in that,
the step of mixing and ball milling zirconia, silicon dioxide, feldspar and 1-2 parts of carbon powder to obtain mixed ceramic powder comprises the following steps:
mixing and ball milling zirconium oxide, silicon dioxide, feldspar and 1-2 parts of carbon powder to obtain mixed ceramic powder, wherein the ball milling time is 3-5h, and the ball milling rotating speed is 200-400rpm to obtain mixed powder II containing the carbon powder.
7. The method for preparing the normal-temperature self-drying high-temperature anti-corrosion nano ceramic coating according to claim 2, which is characterized in that,
the step of carburizing the mixed ceramic powder to obtain the ceramic oxide containing the carburized layer comprises the following steps:
carburizing the mixed ceramic powder, wherein the carburizing temperature is 1000-1400 ℃, the treatment time is 2-4h, the treatment atmosphere is vacuum, and the vacuum degree is 0.1-0.5pa, and finally obtaining the ceramic oxide containing the carburized layer.
8. The method for preparing the normal-temperature self-drying high-temperature anti-corrosion nano ceramic coating according to claim 2, which is characterized in that,
the step of carrying out mixed ball milling treatment on the ceramic oxide containing the carburized layer, cerium oxide, yttrium oxide and lanthanum oxide to obtain a mixture of ceramic powder comprises the following steps:
mixing and ball milling the ceramic oxide containing the carburized layer, cerium oxide, yttrium oxide and lanthanum oxide for 1-3h at 200-400rpm to obtain a mixture of ceramic powder.
9. The method for preparing the normal-temperature self-drying high-temperature anti-corrosion nano ceramic coating according to claim 2, which is characterized in that,
the step of stirring and ultrasonic dispersing the mixture of the ceramic powder and the self-drying slurry to obtain the ceramic coating comprises the following steps:
stirring the mixture of the ceramic powder and the self-drying slurry, and performing ultrasonic dispersion, wherein the stirring speed is 100-200rpm, and the stirring time is 30-60min to obtain the ceramic coating.
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