CN114230372B - Corrosion-resistant high-strength ceramic roller and preparation method thereof - Google Patents
Corrosion-resistant high-strength ceramic roller and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an anti-corrosion high-strength ceramic roller, which comprises a ceramic roller body and an anti-corrosion high-strength coating arranged on the surface of the ceramic roller body; the corrosion-resistant high-strength coating comprises the following components in parts by weight: 55-78 parts of aluminum oxide powder, 22-34 parts of silicon dioxide powder, 10-16 parts of niobium nitride coated scandium boride microspheres, 0.5-2 parts of binder, 1-3 parts of absolute ethyl alcohol and 2-4 parts of deionized water. The invention prepares an anti-corrosion high-strength ceramic roller rod, which is characterized in that a layer of anti-corrosion high-strength coating is arranged on the surface of the conventional quartz ceramic so as to protect the quartz ceramic, and the finally prepared ceramic roller rod has better anti-corrosion performance and high-strength performance. Can also improve the high temperature resistance of the quartz ceramic, and solves the problem that the strength of the quartz ceramic is reduced at the temperature of more than l100 ℃.
Description
Technical Field
The invention relates to the field of ceramic roller rods, in particular to an anti-corrosion high-strength ceramic roller rod and a preparation method thereof.
Background
The quartz ceramic roller is mainly used for a glass high-temperature transmission mechanism of a glass toughening treatment kiln, and has the main advantages that: 1. the heat conductivity coefficient is low, the heat loss is small, and the uniformity of the furnace temperature is high; 2. the hardness is close to that of glass, and the glass cannot be scratched; 3. the material is light, the rigidity is good, and the flatness of the glass can be ensured. Therefore, the quartz ceramic roller is widely used in a tempered glass furnace. The quartz ceramic has the biggest characteristic that the flexural strength and the compressive strength of the quartz ceramic are greatly increased along with the rise of the temperature below l1O0 ℃, but the strength of the quartz ceramic is reduced after the temperature is over 1100 ℃, so that the further development of the quartz ceramic in the metal smelting industry is limited; in addition, a large amount of corrosive gas is generated during high-temperature firing, and the corrosive gas attacks the ceramic roller and reduces the service life of the ceramic roller. Therefore, there is a need for a corrosion resistant, high temperature resistant, and high strength ceramic roll bar.
Disclosure of Invention
Aiming at the problems of limited high temperature resistance, insufficient corrosion resistance and strength to be improved of quartz ceramics in the prior art, the invention aims to provide a corrosion-resistant high-strength ceramic roller and a preparation method thereof.
The purpose of the invention is realized by adopting the following technical scheme:
in a first aspect, the invention provides an anti-corrosion high-strength ceramic roller rod, which comprises a ceramic roller rod body and an anti-corrosion high-strength coating arranged on the surface of the ceramic roller rod body; the corrosion-resistant high-strength coating comprises the following components in parts by weight:
55-78 parts of aluminum oxide powder, 22-34 parts of silicon dioxide powder, 10-16 parts of niobium nitride coated scandium boride microspheres, 0.5-2 parts of binder, 1-3 parts of absolute ethyl alcohol and 2-4 parts of deionized water.
Preferably, the ceramic roller body is prepared by quartz sand with the purity higher than 99.9%.
Preferably, the thickness of the corrosion-resistant high-strength coating is 1-2 mm.
Preferably, the purity of the silica powder is higher than 99.9%, the particle size of the silica powder ranges from 0.5 to 1 μm, from 1 to 5 μm and from 5 to 10 μm; wherein the weight ratio of the particle diameter of 0.5-1 μm to the particle diameter of 1-5 μm to the particle diameter of 5-10 μm is 1.2-1.5.
Preferably, the purity of the aluminium oxide powder is higher than 99.0%, and the grain size of the aluminium oxide powder is in the range of 0.5-1 μm, 1-5 μm and 5-10 μm; wherein the weight ratio of the particle diameter of 0.5-1 μm to the particle diameter of 1-5 μm to the particle diameter of 5-10 μm is 1.2-1.5.
Preferably, the particle size of the niobium nitride coated scandium boride microsphere is 20-50 μm.
Preferably, the binder is polyvinyl alcohol or carboxymethyl cellulose fiber.
Preferably, the preparation process of the niobium nitride coated scandium boride microsphere comprises the following steps:
step one, preparing scandium boride nano powder by using scandium trioxide powder and diboron trioxide powder;
step two, firstly, melamine and formaldehyde are combined with scandium boride nano powder in the reaction process to prepare scandium boride organic composite microspheres;
combining niobium salt and scandium boride organic composite microspheres to obtain niobium/scandium boride organic composite microspheres;
and fourthly, sintering the niobium/scandium boride organic composite microspheres to obtain niobium nitride coated scandium boride microspheres.
Preferably, the process of the first step specifically includes:
s1, weighing and mixing scandium oxide powder and diboron trioxide powder into a ball milling device, adding absolute ethyl alcohol and carboxymethyl cellulose fiber, and carrying out ball milling treatment to obtain mixed slurry; wherein the mass ratio of the scandium oxide powder, the boron oxide powder, the absolute ethyl alcohol and the carboxymethyl cellulose fiber is 1.1-1.3;
s2, carrying out spray drying treatment on the mixed slurry, placing the obtained mixed powder in a high-temperature furnace, heating to 1150-1200 ℃ under the protection of inert gas, carrying out heat preservation treatment for 2-5 h, introducing hydrogen, continuously heating to 1250-1350 ℃, carrying out heat preservation treatment for 2-4 h, and cooling along with the furnace to obtain the scandium boride nano powder.
Preferably, the process of the second step is specifically as follows:
weighing melamine and formaldehyde, mixing the melamine and the formaldehyde into deionized water, fully and uniformly mixing, then adding scandium boride nano powder, ultrasonically dispersing uniformly, heating to 65-80 ℃, stirring for 0.5-1 h, then cooling to room temperature, dropwise adding acetic acid to adjust the pH of the liquid to 4.0-4.5, then stirring for 2-5 h at room temperature, and centrifuging, washing and drying to obtain scandium boride organic composite microspheres; wherein the mass ratio of the melamine, the formaldehyde, the scandium boride nano powder and the deionized water is 1.5-0.75.
Preferably, the process of the third step specifically comprises:
mixing niobium pentachloride and hydrochloric acid, stirring until the niobium pentachloride and the hydrochloric acid are completely dissolved, adding scandium boride organic composite microspheres, performing ultrasonic dispersion treatment for 1-2 hours, stirring at room temperature for 12-24 hours, and freeze-drying to obtain niobium/scandium boride organic composite microspheres; wherein, the concentration of the hydrochloric acid is 0.02-0.05 mol/L, and the mass ratio of the niobium pentachloride and scandium boride organic composite microspheres to the hydrochloric acid is 1.
Preferably, the process of the fourth step is specifically as follows:
placing the niobium/scandium boride organic composite microspheres in a tube furnace, heating to 450-500 ℃ in the atmosphere of air, carrying out heat preservation treatment for 2-4 h, introducing nitrogen as protective gas, heating to 1125-1200 ℃, carrying out heat preservation treatment for 4-6 h, cooling to 550-600 ℃, introducing oxygen again, carrying out heat preservation treatment for 1-2 h, and cooling along with the furnace to obtain the niobium nitride coated scandium boride microspheres.
Preferably, in S1, zirconia balls are used in the ball milling process, the mass ratio of the zirconia balls to the slurry to be ball milled is 1.2-1.6, the ball milling speed is 50-100 rpm, and the ball milling time is 6-10 hours.
In a second aspect, the invention provides a preparation method of a corrosion-resistant high-strength ceramic roller rod, which comprises the following steps:
step 10, preparing a ceramic roller body by using high-purity quartz sand through slip casting;
step 20, weighing the components of the corrosion-resistant high-strength coating according to parts by weight, mixing the components in a ball mill, and ball-milling the components into mixed slurry;
and step 30, coating the mixed slurry on the surface of the ceramic roller body, drying, and sintering to obtain the corrosion-resistant high-strength ceramic roller.
Preferably, in the step 20, zirconia balls are used in the ball milling process, the mass ratio of the zirconia balls to the slurry to be ball milled is 1.2-1.6, the ball milling speed is 50-100 rpm, and the ball milling time is 6-10 h.
Preferably, in the step 30, the drying process is to dry naturally at room temperature and in a shaded place for 10 to 15 hours, and then to dry by heating in a drying oven at 55 to 75 ℃ for 5 to 10 hours.
Preferably, in the step 30, the sintering is to place the dried blank in a sintering furnace, heat up to 500-550 ℃ at a speed of 1-3 ℃/min, then carry out heat preservation treatment for 1-2 h, heat up to 1200-1250 ℃ at a speed of 2-4 ℃/min, then carry out heat preservation treatment for 3-5 h, and naturally cool.
The invention has the beneficial effects that:
the invention prepares an anti-corrosion high-strength ceramic roller rod, which is characterized in that a layer of anti-corrosion high-strength coating is arranged on the surface of the conventional quartz ceramic so as to protect the quartz ceramic, and the finally prepared ceramic roller rod has better anti-corrosion performance and high-strength performance. Can also improve the high temperature resistance of the quartz ceramic, and solves the problem that the strength of the quartz ceramic is reduced at the temperature of more than 1O0 ℃.
The anti-corrosion high-strength coating used in the invention is formed by adding niobium nitride coated scandium boride microspheres on the basis of silicon dioxide and aluminum oxide. The alumina has high mechanical strength, good wear resistance, good corrosion resistance and good thermal stability, the silicon dioxide has good wear resistance, high hardness and low thermal expansion coefficient, but the fusion degree of the alumina and the silicon dioxide is poor, and the phenomenon of low density is easy to occur in the subsequent sintering process. The niobium nitride coated scandium boride microsphere added in the preparation method disclosed by the invention can promote sintering in the process of combining aluminum oxide and silicon dioxide, so that the density is improved, the mechanical strength is improved, and in addition, the wear resistance of the aluminum oxide and silicon dioxide composite material can be improved. The niobium nitride coated scandium boride microsphere is microspherical, has high temperature resistance, can relieve the stress effect, enables the corrosion-resistant high-strength coating to act at high temperature for a long time, and ensures high temperature resistance and mechanical property.
Detailed Description
For the purpose of more clearly illustrating the present invention and more clearly understanding the technical features, objects and advantages of the present invention, the technical solutions of the present invention will now be described in detail below, but the present invention should not be construed as being limited to the implementable scope of the present invention.
In the preparation process of the niobium nitride coated scandium boride microsphere, firstly, scandium trioxide and boron trioxide are ground by a wet method, then, spray drying is carried out to form uniformly mixed powder, and then, high-temperature sintering treatment is carried out to prepare scandium boride nano powder; then, a polymer generated by the reaction of melamine and formaldehyde is used as an organic coating and is combined with the scandium boride nano powder to generate a microspherical structure; then mixing the scandium boride organic composite microspheres with an acid solution of niobium salt, so that niobium ions are uniformly adsorbed on the surfaces and the inner linings of the microspheres; and then sintering the microspheres adsorbed with the niobium ions at high temperature, and finally decomposing the polymer, wherein the niobium ions generate niobium nitride to coat the surfaces of the microspheres.
In the sintering process of the niobium/scandium boride organic composite microsphere, in the atmosphere of air, firstly, heating to 450-500 ℃ to gradually decompose a polymer, wherein part of the polymer is changed into gas to volatilize, and part of the polymer is also converted into carbon, and simultaneously, niobium is combined with oxygen in the air to generate niobium oxide; then introducing nitrogen as a protective gas, simultaneously heating to 1125-1200 ℃, reacting niobium oxide with carbon converted from the nitrogen and the polymer in the process, so that the niobium oxide is completely converted into niobium nitride, and scandium boride in the microspheres is gradually coated in the process, thereby generating scandium boride microspheres coated with niobium nitride; and finally oxygen is again introduced to remove residual carbon.
In the process of preparing the scandium boride organic composite microsphere adsorbed with niobium, the melamine-formaldehyde polymer is partially decomposed in an acid solution to form cyanuric acid, the cyanuric acid belongs to triazine compounds, and has coordination points and can form coordination with metal niobium ions, and meanwhile, the polymer microsphere has certain adsorbability, so that the metal niobium ions can be uniformly and stably combined on the surface of the microsphere, and a coating structure formed for subsequent sintering is used as a bedding.
The invention is further described below with reference to the following examples.
Example 1
An anti-corrosion high-strength ceramic roller comprises a ceramic roller body and an anti-corrosion high-strength coating arranged on the surface of the ceramic roller body; the corrosion-resistant high-strength coating comprises the following components in parts by weight:
64 parts of aluminum oxide powder, 28 parts of silicon dioxide powder, 13 parts of niobium nitride-coated scandium boride microspheres, 1.2 parts of polyvinyl alcohol, 2 parts of absolute ethyl alcohol and 3 parts of deionized water.
Wherein the ceramic roller body is prepared by quartz sand with the purity higher than 99.9%; the thickness of the corrosion-resistant high-strength coating is 1.5mm.
The purity of the silicon dioxide powder is higher than 99.9%, and the particle size of the silicon dioxide powder is in the range of 0.5-1 μm, 1-5 μm and 5-10 μm; wherein the weight ratio of the particle diameter of 0.5-1 μm to the particle diameter of 1-5 μm to the particle diameter of 5-10 μm is 1.3.
The purity of the aluminium oxide powder is higher than 99.0%, and the grain size of the aluminium oxide powder is 0.5-1 μm, 1-5 μm and 5-10 μm; wherein the weight ratio of the 0.5-1 μm particle diameter, 1-5 μm particle diameter and 5-10 μm particle diameter is 1.4.
The grain diameter of the niobium nitride coated scandium boride microsphere is 20-50 mu m.
The preparation process of the niobium nitride coated scandium boride microsphere comprises the following steps:
the method comprises the following steps:
s1, weighing and mixing scandium oxide powder and diboron trioxide powder into a ball milling device, adding absolute ethyl alcohol and carboxymethyl cellulose fiber, and carrying out ball milling treatment to obtain mixed slurry; wherein the mass ratio of the scandium oxide powder to the boron oxide powder to the absolute ethyl alcohol to the carboxymethyl cellulose fiber is 1.2; zirconia balls are used in the ball milling process, the mass ratio of the zirconia balls to the slurry to be ball milled is 1.4, the ball milling speed is 100rpm, and the ball milling time is 10 hours;
s2, carrying out spray drying treatment on the mixed slurry, placing the obtained mixed powder in a high-temperature furnace, heating to 1200 ℃ under the protection of inert gas, carrying out heat preservation treatment for 4 hours, introducing hydrogen, continuing heating to 1300 ℃, carrying out heat preservation treatment for 3 hours, and carrying out furnace cooling to obtain scandium boride nano powder.
Step two:
weighing melamine and formaldehyde, mixing the melamine and the formaldehyde into deionized water, fully and uniformly mixing, then adding scandium boride nano powder, performing ultrasonic dispersion uniformly, heating to 70 ℃, performing stirring treatment for 1h, then cooling to room temperature, dropwise adding acetic acid to adjust the pH value of the liquid to 4.0-4.5, then performing stirring treatment for 3h at room temperature, and performing centrifugation, washing and drying treatment to obtain scandium boride organic composite microspheres; wherein the mass ratio of the melamine, the formaldehyde, the scandium boride nano powder and the deionized water is 1.6.
Step three:
mixing niobium pentachloride and hydrochloric acid, stirring until the niobium pentachloride and the hydrochloric acid are completely dissolved, adding scandium boride organic composite microspheres, performing ultrasonic dispersion treatment for 1.5 hours, stirring at room temperature for 24 hours, and freeze-drying to obtain niobium/scandium boride organic composite microspheres; wherein the concentration of the hydrochloric acid is 0.05mol/L, and the mass ratio of the niobium pentachloride and scandium boride organic composite microspheres to the hydrochloric acid is 1.
The process of the fourth step is specifically as follows:
placing the niobium/scandium boride organic composite microspheres in a tube furnace, heating to 500 ℃ in the atmosphere of air, carrying out heat preservation treatment for 3h, introducing nitrogen as a protective gas, heating to 1200 ℃, carrying out heat preservation treatment for 5h, cooling to 600 ℃, introducing oxygen again, carrying out heat preservation treatment for 2h, and cooling along with the furnace to obtain the niobium nitride coated scandium boride microspheres.
The preparation method of the corrosion-resistant high-strength ceramic roller rod comprises the following steps:
step 10, preparing a ceramic roller body by using high-purity quartz sand through slip casting;
step 20, weighing the components of the corrosion-resistant high-strength coating according to parts by weight, mixing the components in a ball mill, and ball-milling the components into mixed slurry; wherein, zirconia balls are used in the ball milling process, the mass ratio of the zirconia balls to the slurry to be ball milled is 1.4, the ball milling speed is 100rpm, and the ball milling time is 10 hours;
step 30, coating the mixed slurry on the surface of the ceramic roller body, drying and sintering to obtain the corrosion-resistant high-strength ceramic roller; the drying treatment is to naturally dry the blank at room temperature and in a shading place for 12 hours, then to heat and dry the blank in a drying box at 60 ℃ for 8 hours, the sintering is to place the dried blank in a sintering furnace, to heat up to 550 ℃ at the speed of 2 ℃/min, then to heat-preservation treatment for 2 hours, to heat up to 1250 ℃ at the speed of 3 ℃/min, then to heat-preservation treatment for 4 hours, and to naturally cool the blank.
Example 2
An anti-corrosion high-strength ceramic roller comprises a ceramic roller body and an anti-corrosion high-strength coating arranged on the surface of the ceramic roller body; the corrosion-resistant high-strength coating comprises the following components in parts by weight:
55 parts of aluminum oxide powder, 22 parts of silicon dioxide powder, 10 parts of niobium nitride-coated scandium boride microspheres, 0.5 part of carboxymethyl cellulose fibers, 1 part of anhydrous ethanol and 2 parts of deionized water.
Wherein the ceramic roller body is prepared by quartz sand with the purity higher than 99.9%; the thickness of the corrosion-resistant high-strength coating is 1mm.
The purity of the silicon dioxide powder is higher than 99.9%, and the particle size of the silicon dioxide powder is in the range of 0.5-1 μm, 1-5 μm and 5-10 μm; wherein the weight ratio of the 0.5-1 μm particle diameter, the 1-5 μm particle diameter and the 5-10 μm particle diameter is 1.2.
The purity of the aluminium oxide powder is higher than 99.0%, and the grain size of the aluminium oxide powder is 0.5-1 μm, 1-5 μm and 5-10 μm; wherein the weight ratio of the 0.5-1 μm particle diameter, the 1-5 μm particle diameter and the 5-10 μm particle diameter is 1.2.
The grain diameter of the niobium nitride coated scandium boride microsphere is 20-50 mu m.
The preparation process of the niobium nitride coated scandium boride microsphere comprises the following steps:
the method comprises the following steps:
s1, weighing and mixing scandium oxide powder and diboron trioxide powder into a ball milling device, adding absolute ethyl alcohol and carboxymethyl cellulose fiber, and carrying out ball milling treatment to obtain mixed slurry; wherein the mass ratio of the scandium oxide powder to the boron oxide powder to the absolute ethyl alcohol to the carboxymethyl cellulose fiber is 1.1; zirconia balls are used in the ball milling process, the mass ratio of the zirconia balls to the slurry to be ball milled is 1.2, the ball milling speed is 50rpm, and the ball milling time is 6 hours;
s2, carrying out spray drying treatment on the mixed slurry, placing the obtained mixed powder in a high-temperature furnace, heating to 1150 ℃ under the protection of inert gas, carrying out heat preservation treatment for 2h, introducing hydrogen, continuously heating to 1250 ℃, carrying out heat preservation treatment for 2h, and cooling along with the furnace to obtain the scandium boride nano powder.
Step two:
weighing melamine and formaldehyde, mixing the melamine and the formaldehyde into deionized water, fully and uniformly mixing, then adding scandium boride nano powder, performing ultrasonic dispersion uniformly, heating to 65 ℃, stirring for 0.5h, then cooling to room temperature, dropwise adding acetic acid to adjust the pH of the liquid to 4.0-4.5, then stirring for 2h at room temperature, and performing centrifugation, washing and drying to obtain scandium boride organic composite microspheres; the mass ratio of melamine, formaldehyde, scandium boride nano powder to deionized water is 1.5.
Step three:
mixing niobium pentachloride and hydrochloric acid, stirring until the niobium pentachloride and the hydrochloric acid are completely dissolved, adding scandium boride organic composite microspheres, performing ultrasonic dispersion treatment for 1 hour, stirring at room temperature for 12 hours, and freeze-drying to obtain niobium/scandium boride organic composite microspheres; wherein, the concentration of the hydrochloric acid is 0.02mol/L, and the mass ratio of the niobium pentachloride and scandium boride organic composite microspheres to the hydrochloric acid is 1.
Step four:
placing the niobium/scandium boride organic composite microspheres in a tube furnace, heating to 450 ℃ in the atmosphere of air, carrying out heat preservation treatment for 2h, introducing nitrogen as a protective gas, heating to 1125 ℃, carrying out heat preservation treatment for 4h, cooling to 550 ℃, introducing oxygen again, carrying out heat preservation treatment for 1h, and cooling along with the furnace to obtain the niobium nitride coated scandium boride microspheres.
The preparation method of the corrosion-resistant high-strength ceramic roller rod comprises the following steps:
step 10, preparing a ceramic roller body by using high-purity quartz sand through slip casting;
step 20, weighing the components of the corrosion-resistant high-strength coating according to parts by weight, mixing the components in a ball mill, and ball-milling the components into mixed slurry; wherein, zirconia balls are used in the ball milling process, the mass ratio of the zirconia balls to the slurry to be ball milled is 1.2, the ball milling speed is 50rpm, and the ball milling time is 6h;
step 30, coating the mixed slurry on the surface of the ceramic roller body, drying and sintering to obtain the corrosion-resistant high-strength ceramic roller; the drying treatment is to naturally dry the blank at room temperature and in a shading place for 10 hours, then to heat and dry the blank in a drying box at 55 ℃ for 5 hours, the sintering treatment is to place the dried blank in a sintering furnace, to heat up to 500 ℃ at the speed of 1 ℃/min, then to heat-preserve for 1 hour, to heat up to 1200 ℃ at the speed of 2 ℃/min, to heat-preserve for 3 hours, and to naturally cool the blank.
Example 3
An anti-corrosion high-strength ceramic roller comprises a ceramic roller body and an anti-corrosion high-strength coating arranged on the surface of the ceramic roller body; the corrosion-resistant high-strength coating comprises the following components in parts by weight:
78 parts of aluminum oxide powder, 34 parts of silicon dioxide powder, 16 parts of niobium nitride coated scandium boride microspheres, 2 parts of polyvinyl alcohol, 3 parts of absolute ethyl alcohol and 4 parts of deionized water.
The ceramic roller body is prepared by quartz sand with the purity higher than 99.9 percent.
The thickness of the corrosion-resistant high-strength coating is 2mm.
The purity of the silicon dioxide powder is higher than 99.9%, and the particle size of the silicon dioxide powder is in the range of 0.5-1 μm, 1-5 μm and 5-10 μm; wherein the weight ratio of the particle diameter of 0.5-1 μm to the particle diameter of 1-5 μm to the particle diameter of 5-10 μm is 1.5.
The purity of the aluminium oxide powder is higher than 99.0%, and the grain size of the aluminium oxide powder is 0.5-1 μm, 1-5 μm and 5-10 μm; wherein the weight ratio of the particle diameter of 0.5-1 μm to the particle diameter of 1-5 μm to the particle diameter of 5-10 μm is 1.5.
The grain diameter of the niobium nitride coated scandium boride microsphere is 20-50 mu m.
The preparation process of the niobium nitride coated scandium boride microsphere comprises the following steps:
the method comprises the following steps:
s1, weighing and mixing scandium oxide powder and diboron trioxide powder into a ball milling device, adding absolute ethyl alcohol and carboxymethyl cellulose fiber, and carrying out ball milling treatment to obtain mixed slurry; wherein the mass ratio of the scandium oxide powder to the boron oxide powder to the absolute ethyl alcohol to the carboxymethyl cellulose fiber is 1.3; zirconia balls are used in the ball milling process, the mass ratio of the zirconia balls to the slurry to be ball milled is 1.6, the ball milling speed is 100rpm, and the ball milling time is 10 hours;
s2, carrying out spray drying treatment on the mixed slurry, placing the obtained mixed powder in a high-temperature furnace, heating to 1200 ℃ under the protection of inert gas, carrying out heat preservation treatment for 5 hours, introducing hydrogen, continuously heating to 1350 ℃, carrying out heat preservation treatment for 4 hours, and cooling along with the furnace to obtain the scandium boride nano powder.
Step two:
weighing melamine and formaldehyde, mixing the melamine and the formaldehyde into deionized water, fully and uniformly mixing, then adding scandium boride nano powder, performing ultrasonic dispersion uniformly, heating to 80 ℃, stirring for 1h, cooling to room temperature, dropwise adding acetic acid to adjust the pH value of the liquid to 4.0-4.5, then stirring for 5h at room temperature, and performing centrifugation, washing and drying to obtain scandium boride organic composite microspheres; the mass ratio of the melamine, the formaldehyde, the scandium boride nano powder to the deionized water is 1.75.
Step three:
mixing niobium pentachloride and hydrochloric acid, stirring until the niobium pentachloride and the hydrochloric acid are completely dissolved, adding scandium boride organic composite microspheres, performing ultrasonic dispersion treatment for 2 hours, stirring at room temperature for 24 hours, and freeze-drying to obtain niobium/scandium boride organic composite microspheres; wherein, the concentration of the hydrochloric acid is 0.05mol/L, and the mass ratio of the niobium pentachloride and scandium boride organic composite microspheres to the hydrochloric acid is 1.
Step four:
placing the niobium/scandium boride organic composite microspheres in a tube furnace, heating to 500 ℃ in the atmosphere of air, carrying out heat preservation treatment for 4 hours, introducing nitrogen as a protective gas, heating to 1200 ℃, carrying out heat preservation treatment for 6 hours, cooling to 600 ℃, introducing oxygen again, carrying out heat preservation treatment for 2 hours, and cooling along with the furnace to obtain niobium nitride coated scandium boride microspheres.
The preparation method of the corrosion-resistant high-strength ceramic roller rod comprises the following steps:
step 10, preparing a ceramic roller body by using high-purity quartz sand through slip casting;
step 20, weighing the components of the corrosion-resistant high-strength coating according to parts by weight, mixing the components in a ball mill, and ball-milling the components into mixed slurry; wherein, zirconia balls are used in the ball milling process, the mass ratio of the zirconia balls to the slurry to be ball milled is 1.6, the ball milling speed is 100rpm, and the ball milling time is 10 hours;
step 30, coating the mixed slurry on the surface of the ceramic roller body, drying and sintering to obtain the corrosion-resistant high-strength ceramic roller; the drying treatment is to naturally dry the blank at room temperature and in a shaded position for 15 hours, then to heat and dry the blank in a drying box at 75 ℃ for 10 hours, the sintering treatment is to place the dried blank in a sintering furnace, to heat up to 550 ℃ at the speed of 3 ℃/min, then to heat-preservation treatment for 2 hours, to heat up to 1250 ℃ at the speed of 4 ℃/min, then to heat-preservation treatment for 5 hours, and to naturally cool the blank.
Comparative example 1
An anti-corrosion high-strength ceramic roller comprises a ceramic roller body and an anti-corrosion high-strength coating arranged on the surface of the ceramic roller body; the corrosion-resistant high-strength coating comprises the following components in parts by weight:
64 parts of aluminum oxide powder, 28 parts of silicon dioxide powder, 13 parts of niobium nitride microspheres, 1.2 parts of polyvinyl alcohol, 2 parts of absolute ethyl alcohol and 3 parts of deionized water.
Wherein the ceramic roller body is prepared by quartz sand with the purity higher than 99.9%; the thickness of the corrosion-resistant high-strength coating is 1.5mm.
The purity of the silicon dioxide powder is higher than 99.9%, and the particle size of the silicon dioxide powder is in the range of 0.5-1 μm, 1-5 μm and 5-10 μm; wherein the weight ratio of the particle diameter of 0.5-1 μm to the particle diameter of 1-5 μm to the particle diameter of 5-10 μm is 1.3.
The purity of the aluminium oxide powder is higher than 99.0%, and the grain size of the aluminium oxide powder is 0.5-1 μm, 1-5 μm and 5-10 μm; wherein the weight ratio of the 0.5-1 μm particle diameter, the 1-5 μm particle diameter and the 5-10 μm particle diameter is 1.4.
The grain diameter of the niobium nitride microspheres is 20-50 mu m.
The preparation method of the corrosion-resistant high-strength ceramic roller rod comprises the following steps:
step 10, preparing a ceramic roller body by using high-purity quartz sand through slip casting;
step 20, weighing the components of the corrosion-resistant high-strength coating according to parts by weight, mixing the components in a ball mill, and ball-milling the components into mixed slurry; wherein, zirconia balls are used in the ball milling process, the mass ratio of the zirconia balls to the slurry to be ball milled is 1.4, the ball milling speed is 100rpm, and the ball milling time is 10 hours;
step 30, coating the mixed slurry on the surface of the ceramic roller body, drying and sintering to obtain the corrosion-resistant high-strength ceramic roller; the drying treatment is to naturally dry the blank at room temperature and in a shading place for 12 hours, then to heat and dry the blank in a drying box at 60 ℃ for 8 hours, the sintering is to place the dried blank in a sintering furnace, to heat up to 550 ℃ at the speed of 2 ℃/min, then to heat-preservation treatment for 2 hours, to heat up to 1250 ℃ at the speed of 3 ℃/min, then to heat-preservation treatment for 4 hours, and to naturally cool the blank.
Comparative example 2
An anti-corrosion high-strength ceramic roller comprises a ceramic roller body and an anti-corrosion high-strength coating arranged on the surface of the ceramic roller body; the corrosion-resistant high-strength coating comprises the following components in parts by weight:
64 parts of aluminum oxide powder, 28 parts of silicon dioxide powder, 13 parts of scandium boride microspheres, 1.2 parts of polyvinyl alcohol, 2 parts of absolute ethyl alcohol and 3 parts of deionized water.
Wherein the ceramic roller body is prepared by quartz sand with the purity higher than 99.9%; the thickness of the corrosion-resistant high-strength coating is 1.5mm.
The purity of the silicon dioxide powder is higher than 99.9%, and the particle size of the silicon dioxide powder is in the range of 0.5-1 μm, 1-5 μm and 5-10 μm; wherein the weight ratio of the particle diameter of 0.5-1 μm to the particle diameter of 1-5 μm to the particle diameter of 5-10 μm is 1.3.
The purity of the aluminium oxide powder is higher than 99.0%, and the grain diameter ranges of the aluminium oxide powder are 0.5-1 μm, 1-5 μm and 5-10 μm; wherein the weight ratio of the 0.5-1 μm particle diameter, the 1-5 μm particle diameter and the 5-10 μm particle diameter is 1.4.
The particle size of the scandium boride microsphere is 20-50 mu m.
The preparation method of the corrosion-resistant high-strength ceramic roller rod comprises the following steps:
step 10, preparing a ceramic roller body by using high-purity quartz sand through slip casting;
step 20, weighing the components of the corrosion-resistant high-strength coating according to parts by weight, mixing the components in a ball mill, and ball-milling the components into mixed slurry; wherein, zirconia balls are used in the ball milling process, the mass ratio of the zirconia balls to the slurry to be ball milled is 1.4, the ball milling speed is 100rpm, and the ball milling time is 10 hours;
step 30, coating the mixed slurry on the surface of the ceramic roller body, drying and sintering to obtain the corrosion-resistant high-strength ceramic roller; the drying treatment is to naturally dry the blank at room temperature and in a shading place for 12 hours, then to heat and dry the blank in a drying box at 60 ℃ for 8 hours, the sintering is to place the dried blank in a sintering furnace, to heat up to 550 ℃ at the speed of 2 ℃/min, then to heat-preservation treatment for 2 hours, to heat up to 1250 ℃ at the speed of 3 ℃/min, then to heat-preservation treatment for 4 hours, and to naturally cool the blank.
Comparative example 3
Only one corrosion-resistant high-strength ceramic roll body as described in example 1 was used, which was prepared using quartz sand with a purity of more than 99.9%.
In order to more clearly illustrate the invention, the hollow quartz ceramic roller rods (wall thickness of 1 cm) prepared in examples 1 to 3 and comparative examples 1 to 2 of the invention were compared for performance measurement, and the compressive strength was measured according to the standard GB/T4740-1999; the corrosion resistance is detected according to a standard JC/T2138-2012, the acid corrosion rate is the weight reduction of soaking in 3mol/L sulfuric acid at 80 ℃ for 100h, and the alkali corrosion rate is the weight reduction of soaking in 6mol/L sulfuric acid at 80 ℃ for 100 h.
The results are shown in table 1:
TABLE 1 comparison of the Performance measurements of hollow Quartz ceramic Rollers
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (9)
1. The anti-corrosion high-strength ceramic roller is characterized by comprising a ceramic roller body and an anti-corrosion high-strength coating arranged on the surface of the ceramic roller body; the corrosion-resistant high-strength coating comprises the following components in parts by weight:
55 to 78 parts of aluminum oxide powder, 22 to 34 parts of silicon dioxide powder, 10 to 16 parts of niobium nitride coated scandium boride microspheres, 0.5 to 2 parts of binder, 1~3 parts of absolute ethyl alcohol and 2~4 parts of deionized water;
the preparation process of the niobium nitride coated scandium boride microsphere comprises the following steps:
step one, preparing scandium boride nano powder by using scandium trioxide powder and diboron trioxide powder;
step two, firstly, melamine and formaldehyde are combined with scandium boride nano powder in the reaction process to prepare scandium boride organic composite microspheres;
combining niobium salt and scandium boride organic composite microspheres to obtain niobium/scandium boride organic composite microspheres;
and fourthly, sintering the niobium/scandium boride organic composite microspheres to obtain niobium nitride coated scandium boride microspheres.
2. The corrosion-resistant high-strength ceramic roller of claim 1, wherein the ceramic roller body is prepared by using quartz sand with a purity higher than 99.9%.
3. The corrosion-resistant high-strength ceramic roller rod as claimed in claim 1, wherein the purity of the silicon dioxide powder is higher than 99.9%, and the particle size of the silicon dioxide powder is in the range of 0.5 to 1 μm, 1~5 μm and 5 to 10 μm; wherein the weight ratio of the particle diameter of 0.5 to 1 mu m, the particle diameter of 1~5 mu m and the particle diameter of 5 to 10 mu m is 1.2 to 1.5 to 2.0.
4. The corrosion-resistant high-strength ceramic roller according to claim 1, wherein the purity of the aluminum oxide powder is higher than 99.0%, and the particle size of the aluminum oxide powder ranges from 0.5 to 1 μm, 1~5 μm and 5 to 10 μm; wherein the weight ratio of the particle diameter of 0.5 to 1 μm to the particle diameter of 1~5 μm to the particle diameter of 5 to 10 μm is 1.2 to 1.5 to 2.0.
5. The corrosion-resistant high-strength ceramic roller rod as claimed in claim 1, wherein the binder is polyvinyl alcohol or carboxymethyl cellulose fiber.
6. The method for preparing the corrosion-resistant high-strength ceramic roller rod as claimed in claim 1, which is characterized by comprising the following steps:
step 10, preparing a ceramic roller body by using high-purity quartz sand through slip casting;
step 20, weighing the components of the corrosion-resistant high-strength coating according to parts by weight, mixing the components in a ball mill, and ball-milling the components into mixed slurry;
and step 30, coating the mixed slurry on the surface of the ceramic roller body, drying, and sintering to obtain the corrosion-resistant high-strength ceramic roller.
7. The method for preparing the corrosion-resistant high-strength ceramic roller rod according to claim 6, wherein in the step 20, zirconia balls are used in the ball milling process, the mass ratio of the zirconia balls to the slurry to be ball milled is 1.2-1.6, the ball milling speed is 50-100rpm, and the ball milling time is 6-10h.
8. The method for preparing the corrosion-resistant high-strength ceramic roller rod as claimed in claim 6, wherein in the step 30, the drying treatment is performed by naturally drying the roller rod in a shady place at room temperature for 10 to 15h, and then heating and drying the roller rod in a drying box at 55 to 75 ℃ for 5 to 10h.
9. The method for preparing the corrosion-resistant high-strength ceramic roller stick according to claim 6, wherein in the step 30, the blank after drying treatment is placed in a sintering furnace, the temperature is raised to 500-550 ℃ at the speed of 1~3 ℃/min, then the heat preservation treatment is carried out for 1-2h, the temperature is raised to 1200-1250 ℃ at the speed of 2~4 ℃/min, then the heat preservation treatment is carried out for 3-5h, and the product is obtained after natural cooling.
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