CN119143473A - Environment-friendly ceramic and preparation method thereof - Google Patents
Environment-friendly ceramic and preparation method thereof Download PDFInfo
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Abstract
本发明公开一种环保陶瓷及其制备方法，属于陶瓷领域，方法包括：将高岭土、氧化硼、碳粉、锆、碳酸钡、碳酸钙、硼、硅、钛研磨混合得混合料；将硝酸锌、硝酸锆与分散剂混合得混合液；将混合料与混合液混合得混合浆料；将混合浆料制成胚体；将胚体放在烧结炉升温至560‑720℃在第一处理环境中处理1.5‑4h；将烧结炉升温至880‑1130℃在第二处理环境中处理2‑5h；将烧结炉升温至1280‑1420℃在第三处理环境中处理3‑6h；将烧结炉升温至1530‑1620℃在第四处理环境中处理1‑3h；第一处理环境、第二处理环境、第三处理环境与第四处理环境包括真空或惰性气氛。烧结陶瓷强度高，耐磨性与耐腐蚀性较好。The invention discloses an environmentally friendly ceramic and a preparation method thereof, which belongs to the field of ceramics. The method comprises: grinding and mixing kaolin, boron oxide, carbon powder, zirconium, barium carbonate, calcium carbonate, boron, silicon and titanium to obtain a mixture; mixing zinc nitrate, zirconium nitrate and a dispersant to obtain a mixed solution; mixing the mixture and the mixed solution to obtain a mixed slurry; making the mixed slurry into an embryo; placing the embryo in a sintering furnace and heating it to 560-720°C for 1.5-4h in a first treatment environment; heating the sintering furnace to 880-1130°C for 2-5h in a second treatment environment; heating the sintering furnace to 1280-1420°C for 3-6h in a third treatment environment; heating the sintering furnace to 1530-1620°C for 1-3h in a fourth treatment environment; the first treatment environment, the second treatment environment, the third treatment environment and the fourth treatment environment include a vacuum or an inert atmosphere. The sintered ceramic has high strength and good wear resistance and corrosion resistance.
Description
Technical Field
The invention belongs to the field of ceramics, and particularly relates to an environment-friendly ceramic and a preparation method thereof.
Background
Ceramics have a long history of development, and early ceramics are mainly fired by clay and the like, and the prepared ceramics are mainly used as food appliances, wine wares, ceramic arts and the like. With the development of new materials and material processes, the preparation raw materials and the firing process of the ceramic are changed continuously, so that the performance of the fired ceramic is better, the application field of the ceramic is wider, such as machinery, chemical industry, aerospace and the like, and the performance requirements on the ceramic are higher. In many application fields, the ceramic is required to have higher strength, higher wear resistance and corrosion resistance so as to be suitable for different use environment conditions, the wear resistance of the existing ceramic is poor, the use requirement is difficult to meet, and the application of the ceramic is influenced.
Disclosure of Invention
The invention provides an environment-friendly ceramic and a preparation method thereof, which are used for solving the problem of poor wear resistance of the ceramic.
The invention provides a preparation method of environment-friendly ceramic, which comprises the following steps:
Step S1, grinding and mixing kaolin, boron oxide, carbon powder, zirconium, barium carbonate, calcium carbonate, boron, silicon and titanium to obtain a mixture;
mixing zinc nitrate, zirconium nitrate and a dispersing agent to obtain a mixed solution;
mixing the mixture with the mixed solution to obtain mixed slurry;
S2, preparing the mixed slurry into a blank to be sintered;
s3, placing the blank in a sintering furnace, heating to a first temperature of 560-720 ℃ and treating for 1.5-4h in a first treatment environment;
step S4, heating the sintering furnace from the first temperature 560-720 ℃ to the second temperature 880-1130 ℃ and treating for 2-5h in a second treatment environment;
step S5, heating the sintering furnace from the second temperature 880-1130 ℃ to a third temperature 1280-1420 ℃ and treating for 3-6h in a third treatment environment;
step S6, heating the sintering furnace from the third temperature 1280-1420 ℃ to the fourth temperature 1530-1620 ℃ for 1-3h in a fourth treatment environment;
the first processing environment comprises a vacuum or inert atmosphere, the second processing environment comprises a vacuum or inert atmosphere, the third processing environment comprises a vacuum or inert atmosphere, and the fourth processing environment comprises a vacuum or inert atmosphere.
Further, the raw materials for preparing the ceramic comprise:
12-25 parts of kaolin;
2.5-4.5 parts by weight of boron oxide;
0.5 to 1.3 parts by weight of carbon powder;
Zirconium 0.7-1.6 weight portions;
0.5 to 1.2 parts by weight of barium carbonate;
0.4-0.9 parts by weight of calcium carbonate;
0.3-0.7 parts by weight of zinc nitrate;
zirconium nitrate 0.6-1.8 weight portions;
0.5 to 1.4 parts by weight of boron;
0.4-0.8 parts by weight of silicon;
Titanium 0.3-1.2 weight portions.
Further, the first processing environment is vacuum, the second processing environment comprises nitrogen and argon, the third processing environment comprises nitrogen and argon, and the fourth processing environment is vacuum.
Further, the third treatment environment comprises nitrogen, argon, silane, methane and boron trichloride, wherein the volume of the silane in the third treatment atmosphere is 1.5-4%, the volume of the methane in the third treatment atmosphere is 2-5%, the volume of the boron trichloride in the third treatment environment is 1-3%, and the volume of the nitrogen in the third treatment environment is 8-15%;
The fourth processing environment is vacuum.
Further, the kaolin is modified kaolin, and the preparation method of the modified kaolin comprises the following steps:
placing kaolin into an acidic solution for pickling;
Placing the kaolin subjected to acid washing in a calcium hydroxide solution for mixing treatment;
Then drying to obtain a dried product;
then mixing the dried product with boron oxide, aluminum, carbon powder, silicon and tungsten trioxide to obtain a mixture;
Treating the mixture in vacuum at 620-780 deg.C for 0.5-1.5 hr;
then the mixture is placed in a treatment gas for 2 to 3.5 hours at 1150 to 1320 ℃;
then cooling and grinding to obtain modified kaolin;
The process gas includes nitrogen and argon.
Further, the boron oxide in the mixture is 0.5-0.9% of the mass of the kaolin, the aluminum in the mixture is 0.3-0.7% of the mass of the kaolin, the carbon powder in the mixture is 0.7-1.2% of the mass of the kaolin, the silicon in the mixture is 0.5-1% of the mass of the kaolin, and the tungsten trioxide in the mixture is 0.3-0.8% of the mass of the kaolin.
Further, the volume of nitrogen in the process gas is 12-25%.
Further, the raw materials for preparing the ceramic also comprise:
the preparation method of the modified mullite comprises the following steps:
placing mullite in water at 60-85 ℃ for treatment for 1-2h;
filtering and drying to obtain a filtered substance;
Then mixing the filtrate with titanium boride, zirconium oxide, boron carbide and carbon powder to obtain mixed powder;
placing the mixed powder in vacuum and treating at 950-1160 ℃ for 0.5-1h;
then the mixed powder is placed in modified gas to be treated for 1 to 3 hours at 1220 to 1400 ℃;
Finally, cooling and grinding to obtain modified mullite;
The titanium boride in the mixed powder is 0.5-1% of the mullite mass, the zirconia in the mixed powder is 0.3-0.8% of the mullite mass, the boron carbide in the mixed powder is 0.5-1.3% of the mullite mass, and the carbon powder in the mixed powder is 0.6-1% of the mullite mass;
The modifying gas comprises nitrogen, argon and silane, wherein the volume of the nitrogen in the modifying gas is 7-13%, and the volume of the silane in the modifying gas is 1.2-2.5%.
Further, the content of the modified mullite is 6-11 parts by weight.
The environment-friendly ceramic of the embodiment of the invention is prepared by the preparation method described in the embodiment.
According to the preparation method of the environment-friendly ceramic, kaolin, boron oxide, carbon powder, zirconium, barium carbonate, calcium carbonate, boron, silicon and titanium are ground and mixed to obtain a mixture, zinc nitrate, zirconium nitrate and a dispersing agent are mixed to obtain a mixed solution, and then the mixed solution and the mixed solution are mixed to obtain a mixed slurry, and the mixed slurry is sintered by the method after being prepared into a green body, so that the ceramic prepared by sintering has high mechanical strength, better wear resistance and better corrosion resistance, can be suitable for more use environments, and can meet the use requirements.
Detailed Description
The technical solutions of the embodiments of the present invention will be described below in conjunction with the embodiments of the present invention, and the embodiments described in the present invention are some of the embodiments of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The preparation method of the environment-friendly ceramic provided by the embodiment of the invention comprises the following steps:
Step S1, grinding and mixing kaolin, boron oxide, carbon powder, zirconium, barium carbonate, calcium carbonate, boron, silicon and titanium to obtain a mixture;
mixing zinc nitrate, zirconium nitrate and a dispersing agent to obtain a mixed solution;
mixing the mixture with the mixed solution to obtain mixed slurry;
S2, preparing the mixed slurry into a blank to be sintered;
s3, placing the blank in a sintering furnace, heating to a first temperature of 560-720 ℃ and treating for 1.5-4h in a first treatment environment;
step S4, heating the sintering furnace from the first temperature 560-720 ℃ to the second temperature 880-1130 ℃ and treating for 2-5h in a second treatment environment;
step S5, heating the sintering furnace from the second temperature 880-1130 ℃ to a third temperature 1280-1420 ℃ and treating for 3-6h in a third treatment environment;
step S6, heating the sintering furnace from the third temperature 1280-1420 ℃ to the fourth temperature 1530-1620 ℃ for 1-3h in a fourth treatment environment;
the first processing environment comprises a vacuum or inert atmosphere, the second processing environment comprises a vacuum or inert atmosphere, the third processing environment comprises a vacuum or inert atmosphere, and the fourth processing environment comprises a vacuum or inert atmosphere.
Optionally, the raw materials for preparing the ceramic comprise:
12-25 parts of kaolin;
2.5-4.5 parts by weight of boron oxide;
0.5 to 1.3 parts by weight of carbon powder;
Zirconium 0.7-1.6 weight portions;
0.5 to 1.2 parts by weight of barium carbonate;
0.4-0.9 parts by weight of calcium carbonate;
0.3-0.7 parts by weight of zinc nitrate;
zirconium nitrate 0.6-1.8 weight portions;
0.5 to 1.4 parts by weight of boron;
0.4-0.8 parts by weight of silicon;
Titanium 0.3-1.2 weight portions.
For example, the raw materials for preparing the ceramic can comprise 12 parts by weight of kaolin, 2.5 parts by weight of boron oxide, 1.3 parts by weight of carbon powder, 0.7 part by weight of zirconium, 1.2 parts by weight of barium carbonate, 0.4 part by weight of calcium carbonate, 0.3 part by weight of zinc nitrate, 1.8 parts by weight of zirconium nitrate, 0.5 part by weight of boron, 0.4 part by weight of silicon and 1.2 parts by weight of titanium, and the dosage of the specific components can be adjusted according to requirements.
Optionally, the first processing environment is vacuum, the second processing environment comprises nitrogen and argon, the third processing environment comprises nitrogen and argon, and the fourth processing environment is vacuum.
In the embodiment of the invention, the third treatment environment comprises nitrogen, argon, silane, methane and boron trichloride, the volume of the silane in the third treatment atmosphere is 1.5-4%, the volume of the methane in the third treatment atmosphere is 2-5%, the volume of the boron trichloride in the third treatment environment is 1-3%, the volume of the nitrogen in the third treatment environment is 8-15%, and the fourth treatment environment is vacuum. For example, the third treatment environment includes nitrogen, argon, silane, methane, and boron trichloride, the volume of silane in the third treatment atmosphere is 1.5%, the volume of methane in the third treatment atmosphere is 5%, the volume of boron trichloride in the third treatment environment is 3%, the volume of nitrogen in the third treatment environment is 8%, and the fourth treatment environment is vacuum, and the specific gas composition and volume can be adjusted as required.
In some embodiments of the invention, the kaolin may be a modified kaolin, and the method of preparing the modified kaolin may include:
placing kaolin into an acidic solution for pickling;
Placing the kaolin subjected to acid washing in a calcium hydroxide solution for mixing treatment;
Then drying to obtain a dried product;
then mixing the dried product with boron oxide, aluminum, carbon powder, silicon and tungsten trioxide to obtain a mixture;
Treating the mixture in vacuum at 620-780 deg.C for 0.5-1.5 hr;
then the mixture is placed in a treatment gas for 2 to 3.5 hours at 1150 to 1320 ℃;
then cooling and grinding to obtain modified kaolin;
The process gas includes nitrogen and argon.
The acidic solution may be a nitric acid solution, an oxalic acid solution, a hydrochloric acid solution, etc., and the acidic solution may be a nitric acid solution of 0.3 to 1mol/L, for example, the acidic solution may be a nitric acid solution of 0.5 mol/L. The mass content of calcium hydroxide in the calcium hydroxide solution is 5 to 10%, for example, the mass content of calcium hydroxide in the calcium hydroxide solution is 5%. The drying process can be performed under vacuum environment of 60-90deg.C.
Optionally, the boron oxide in the mixture is 0.5-0.9% of the mass of the kaolin, the aluminum in the mixture is 0.3-0.7% of the mass of the kaolin, the carbon powder in the mixture is 0.7-1.2% of the mass of the kaolin, the silicon in the mixture is 0.5-1% of the mass of the kaolin, and the tungsten trioxide in the mixture is 0.3-0.8% of the mass of the kaolin. The volume of nitrogen in the process gas is 12-25%. For example, the boron oxide in the mixture is 0.5% of the kaolin mass, the aluminum in the mixture is 0.7% of the kaolin mass, the carbon powder in the mixture is 0.7% of the kaolin mass, the silicon in the mixture is 1% of the kaolin mass, and the tungsten trioxide in the mixture is 0.8% of the kaolin mass. The volume of nitrogen in the process gas was 12%.
In some embodiments, the raw materials for preparing the ceramic may further include:
modified mullite, the preparation method of modified mullite can include:
placing mullite in water at 60-85 ℃ for treatment for 1-2h;
Filtering and drying to obtain filtrate, wherein the filtrate can be dried in a vacuum environment at 65-85deg.C;
Then mixing the filtrate with titanium boride, zirconium oxide, boron carbide and carbon powder to obtain mixed powder;
placing the mixed powder in vacuum and treating at 950-1160 ℃ for 0.5-1h;
then the mixed powder is placed in modified gas to be treated for 1 to 3 hours at 1220 to 1400 ℃;
Finally, cooling and grinding to obtain modified mullite;
The titanium boride in the mixed powder is 0.5-1% of the mullite mass, the zirconia in the mixed powder is 0.3-0.8% of the mullite mass, the boron carbide in the mixed powder is 0.5-1.3% of the mullite mass, and the carbon powder in the mixed powder is 0.6-1% of the mullite mass;
The modifying gas comprises nitrogen, argon and silane, wherein the volume of the nitrogen in the modifying gas is 7-13%, and the volume of the silane in the modifying gas is 1.2-2.5%.
For example, mullite is placed in 75 ℃ water for 1.5 hours, filtered and dried to obtain a filtered material, then the filtered material is mixed with titanium boride, zirconium oxide, boron carbide and carbon powder to obtain mixed powder, the mixed powder is placed in vacuum for 1 hour at 950 ℃, the mixed powder is placed in modified gas for 3 hours at 1220 ℃, finally the mixed powder is ground after cooling to obtain modified mullite, the titanium boride in the mixed powder is 0.5% of mullite mass, the zirconium oxide in the mixed powder is 0.8% of mullite mass, the boron carbide in the mixed powder is 0.5% of mullite mass, the carbon powder in the mixed powder is 1% of mullite mass, the modified gas comprises nitrogen, argon and silane, the volume of nitrogen in the modified gas is 7%, and the volume of silane in the modified gas is 2.5%.
Optionally, the modified mullite is present in an amount of 6 to 11 parts by weight. For example, the modified mullite is contained in an amount of 6, 9 or 11 parts by weight.
The environment-friendly ceramic of the embodiment of the invention is prepared by the preparation method described in the embodiment.
The invention will now be illustrated by means of some examples.
Example 1
The raw materials comprise:
12 parts of kaolin and 2.5 parts of boron oxide;
0.5 part by weight of carbon powder and 1.6 parts by weight of zirconium;
0.5 parts by weight of barium carbonate and 0.4 parts by weight of calcium carbonate;
0.3 parts of zinc nitrate and 1.8 parts of zirconium nitrate;
1.4 parts by weight of boron, 0.4 part by weight of silicon and 1.2 parts by weight of titanium;
the preparation method of the environment-friendly ceramic comprises the following steps:
Step S1, grinding and mixing kaolin, boron oxide, carbon powder, zirconium, barium carbonate, calcium carbonate, boron, silicon and titanium to obtain a mixture;
mixing zinc nitrate, zirconium nitrate and a dispersing agent to obtain a mixed solution;
mixing the mixture with the mixed solution to obtain mixed slurry;
S2, preparing the mixed slurry into a blank to be sintered;
Step S3, placing the blank in a sintering furnace, heating to a first temperature 560, and treating for 4 hours in a first treatment environment;
step S4, heating the sintering furnace from the first temperature of 560 ℃ to the second temperature of 1130 ℃ for 2 hours in a second treatment environment;
step S5, heating the sintering furnace from the second temperature 1130 ℃ to a third temperature 1280 ℃ and treating for 6 hours in a third treatment environment;
step S6, heating the sintering furnace from the third temperature 1280 ℃ to the fourth temperature 1530 ℃ and treating for 1h in a fourth treatment environment;
the dispersing agent is a mixed solution of water and ethanol, the volume ratio of the water to the ethanol is 1:3, the first treatment environment is vacuum, the second treatment environment is vacuum, the third treatment environment is vacuum, and the fourth treatment environment is vacuum.
Example 2
The raw materials comprise:
25 parts of kaolin and 4.5 parts of boron oxide;
1.3 parts of carbon powder and 0.7 part of zirconium;
1.2 parts of barium carbonate and 0.9 part of calcium carbonate;
0.7 parts of zinc nitrate and 0.6 parts of zirconium nitrate;
0.5 part by weight of boron, 0.8 part by weight of silicon and 0.3 part by weight of titanium;
the preparation method of the environment-friendly ceramic comprises the following steps:
Step S1, grinding and mixing kaolin, boron oxide, carbon powder, zirconium, barium carbonate, calcium carbonate, boron, silicon and titanium to obtain a mixture;
mixing zinc nitrate, zirconium nitrate and a dispersing agent to obtain a mixed solution;
mixing the mixture with the mixed solution to obtain mixed slurry;
S2, preparing the mixed slurry into a blank to be sintered;
Step S3, placing the blank in a sintering furnace, heating to a first temperature of 720 ℃ and treating for 1.5h in a first treatment environment;
Step S4, heating the sintering furnace from the first temperature 720 ℃ to the second temperature 880 ℃ and treating for 5 hours in a second treatment environment;
Step S5, heating the sintering furnace from the second temperature 880 ℃ to a third temperature 1420 ℃ and treating for 3 hours in a third treatment environment;
Step S6, heating the sintering furnace from the third temperature 1420 ℃ to the fourth temperature 1620 ℃ for 3 hours in a fourth treatment environment;
the dispersing agent is a mixed solution of water and ethanol, the volume ratio of the water to the ethanol is 1:3, the first treatment environment is vacuum, the second treatment environment is vacuum, the third treatment environment is vacuum, and the fourth treatment environment is vacuum.
Example 3
The raw materials comprise:
18 parts of kaolin and 3.5 parts of boron oxide;
0.9 weight part of carbon powder and 1.2 weight parts of zirconium;
0.8 parts by weight of barium carbonate and 0.7 parts by weight of calcium carbonate;
0.5 part by weight of zinc nitrate and 1.2 parts by weight of zirconium nitrate;
0.9 parts by weight of boron, 0.6 parts by weight of silicon and 0.7 parts by weight of titanium;
the preparation method of the environment-friendly ceramic comprises the following steps:
Step S1, grinding and mixing kaolin, boron oxide, carbon powder, zirconium, barium carbonate, calcium carbonate, boron, silicon and titanium to obtain a mixture;
mixing zinc nitrate, zirconium nitrate and a dispersing agent to obtain a mixed solution;
mixing the mixture with the mixed solution to obtain mixed slurry;
S2, preparing the mixed slurry into a blank to be sintered;
Step S3, placing the blank in a sintering furnace, heating to a first temperature of 620 ℃ and treating for 3 hours in a first treatment environment;
Step S4, heating the sintering furnace from the first temperature of 620 ℃ to the second temperature of 1020 ℃ and treating for 3 hours in a second treatment environment;
Step S5, heating the sintering furnace from the second temperature of 1020 ℃ to a third temperature of 1350 ℃ and treating for 4 hours in a third treatment environment;
Step S6, heating the sintering furnace from the third temperature 1350 ℃ to a fourth temperature 1580 ℃ for 2 hours in a fourth treatment environment;
the dispersing agent is a mixed solution of water and ethanol, the volume ratio of the water to the ethanol is 1:3, the first treatment environment is vacuum, the second treatment environment is vacuum, the third treatment environment is vacuum, and the fourth treatment environment is vacuum.
Example 4
Example 4 differs from example 3 in that:
The third treatment environment comprises nitrogen, argon, silane, methane and boron trichloride, wherein the volume of the silane in the third treatment atmosphere is 1.5%, the volume of the methane in the third treatment atmosphere is 5%, the volume of the boron trichloride in the third treatment environment is 1%, the volume of the nitrogen in the third treatment environment is 8%, and the fourth treatment environment is vacuum.
Example 5
Example 5 differs from example 3 in that:
The third treatment environment comprises nitrogen, argon, silane, methane and boron trichloride, wherein the volume of the silane in the third treatment atmosphere is 4%, the volume of the methane in the third treatment atmosphere is 2%, the volume of the boron trichloride in the third treatment environment is 3%, the volume of the nitrogen in the third treatment environment is 15%, and the fourth treatment environment is vacuum.
Example 6
Example 6 differs from example 3 in that:
The kaolin is modified kaolin, and the preparation method of the modified kaolin comprises the following steps:
Placing kaolin into an acidic solution for pickling, wherein the acidic solution is nitric acid solution with the concentration of 0.5 mol/L;
Placing the kaolin subjected to acid washing in a calcium hydroxide solution for mixing treatment, wherein the mass concentration of calcium hydroxide in the calcium hydroxide solution is 5%;
Then drying at 60 ℃ to obtain a dried product;
then mixing the dried product with boron oxide, aluminum, carbon powder, silicon and tungsten trioxide to obtain a mixture;
the mixture was treated in vacuo at 620 ℃ for 1.5h;
the mixture was then placed in a process gas and treated at 1320 ℃ for 2 hours;
then cooling and grinding to obtain modified kaolin;
the processing gas comprises nitrogen and argon, and the volume of the nitrogen in the processing gas is 12%;
The boron oxide in the mixture is 0.5% of the kaolin, the aluminum in the mixture is 0.7% of the kaolin, the carbon powder in the mixture is 0.7% of the kaolin, the silicon in the mixture is 1% of the kaolin, and the tungsten trioxide in the mixture is 0.3% of the kaolin.
Example 7
Example 7 differs from example 3 in that:
The kaolin is modified kaolin, and the preparation method of the modified kaolin comprises the following steps:
Placing kaolin into an acidic solution for pickling, wherein the acidic solution is nitric acid solution with the concentration of 0.8 mol/L;
placing the kaolin subjected to acid washing in a calcium hydroxide solution for mixing treatment, wherein the mass concentration of calcium hydroxide in the calcium hydroxide solution is 7%;
drying at 80 ℃ to obtain a dried product;
then mixing the dried product with boron oxide, aluminum, carbon powder, silicon and tungsten trioxide to obtain a mixture;
the mixture was treated in vacuo at 780 ℃ for 0.5h;
the mixture was then placed in a process gas and treated at 1150 ℃ for 3.5h;
then cooling and grinding to obtain modified kaolin;
the processing gas comprises nitrogen and argon, and the volume of the nitrogen in the processing gas is 25%;
the boron oxide in the mixture is 0.9% of the kaolin, the aluminum in the mixture is 0.3% of the kaolin, the carbon powder in the mixture is 1.2% of the kaolin, the silicon in the mixture is 0.5% of the kaolin, and the tungsten trioxide in the mixture is 0.8% of the kaolin.
Example 8
Example 8 differs from example 3 in that:
the raw materials for preparing the ceramic also comprise:
The modified mullite comprises 6 parts by weight of modified mullite, and the preparation method of the modified mullite comprises the following steps:
placing mullite in water at 60 ℃ for 2 hours;
drying at 65 ℃ after filtering to obtain a filtered substance;
Then mixing the filtrate with titanium boride, zirconium oxide, boron carbide and carbon powder to obtain mixed powder;
the mixed powder is placed in vacuum for treatment at 950 ℃ for 1h;
Then the mixed powder is placed in modified gas to be treated for 1h at 1400 ℃;
Finally, cooling and grinding to obtain modified mullite;
The titanium boride in the mixed powder is 0.5% of the mullite, the zirconia in the mixed powder is 0.8% of the mullite, the boron carbide in the mixed powder is 1.3% of the mullite, and the carbon powder in the mixed powder is 0.6% of the mullite;
the modifying gas comprises nitrogen, argon and silane, wherein the volume of the nitrogen in the modifying gas is 7%, and the volume of the silane in the modifying gas is 2.5%.
Example 9
Example 9 differs from example 3 in that:
the raw materials for preparing the ceramic also comprise:
The modified mullite comprises 11 parts by weight of modified mullite, and the preparation method of the modified mullite comprises the following steps:
Placing mullite in 75 ℃ water for treatment for 1h;
drying at 80 ℃ after filtering to obtain a filtered substance;
Then mixing the filtrate with titanium boride, zirconium oxide, boron carbide and carbon powder to obtain mixed powder;
placing the mixed powder in vacuum and treating at 1160 ℃ for 0.5h;
Then placing the mixed powder in modified gas and treating for 3 hours at 1220 ℃;
Finally, cooling and grinding to obtain modified mullite;
the titanium boride in the mixed powder is 1% of the mullite, the zirconium oxide in the mixed powder is 0.3% of the mullite, the boron carbide in the mixed powder is 0.5% of the mullite, and the carbon powder in the mixed powder is 1% of the mullite;
the modifying gas comprises nitrogen, argon and silane, wherein the volume of the nitrogen in the modifying gas is 13%, and the volume of the silane in the modifying gas is 1.2%.
Example 10
Example 10 differs from example 7 in that:
the raw materials for preparing the ceramic also comprise:
The modified mullite comprises 6 parts by weight of modified mullite, and the preparation method of the modified mullite comprises the following steps:
placing mullite in water at 60 ℃ for 2 hours;
drying at 65 ℃ after filtering to obtain a filtered substance;
Then mixing the filtrate with titanium boride, zirconium oxide, boron carbide and carbon powder to obtain mixed powder;
the mixed powder is placed in vacuum for treatment at 950 ℃ for 1h;
Then the mixed powder is placed in modified gas to be treated for 1h at 1400 ℃;
Finally, cooling and grinding to obtain modified mullite;
The titanium boride in the mixed powder is 0.5% of the mullite, the zirconia in the mixed powder is 0.8% of the mullite, the boron carbide in the mixed powder is 1.3% of the mullite, and the carbon powder in the mixed powder is 0.6% of the mullite;
the modifying gas comprises nitrogen, argon and silane, wherein the volume of the nitrogen in the modifying gas is 7%, and the volume of the silane in the modifying gas is 2.5%.
Example 11
Example 11 differs from example 7 in that:
the raw materials for preparing the ceramic also comprise:
The modified mullite comprises 11 parts by weight of modified mullite, and the preparation method of the modified mullite comprises the following steps:
Placing mullite in 75 ℃ water for treatment for 1h;
drying at 80 ℃ after filtering to obtain a filtered substance;
Then mixing the filtrate with titanium boride, zirconium oxide, boron carbide and carbon powder to obtain mixed powder;
placing the mixed powder in vacuum and treating at 1160 ℃ for 0.5h;
Then placing the mixed powder in modified gas and treating for 3 hours at 1220 ℃;
Finally, cooling and grinding to obtain modified mullite;
the titanium boride in the mixed powder is 1% of the mullite, the zirconium oxide in the mixed powder is 0.3% of the mullite, the boron carbide in the mixed powder is 0.5% of the mullite, and the carbon powder in the mixed powder is 1% of the mullite;
the modifying gas comprises nitrogen, argon and silane, wherein the volume of the nitrogen in the modifying gas is 13%, and the volume of the silane in the modifying gas is 1.2%.
The ceramics prepared in the above examples were tested and the specific test results are shown in table 1.
Corrosion resistance test of ceramics:
1. And (3) acid resistance test, namely cleaning the ceramic with deionized water, drying, weighing the ceramic, observing the surface condition, soaking the ceramic in nitric acid solution with the concentration of 0.6mol/L at 50 ℃ for 150 hours, taking out, cleaning with deionized water, drying, weighing the ceramic again, and comparing the quality with the change before and after.
2. And (3) alkali resistance testing, namely cleaning and drying the ceramic by using deionized water, weighing the quality of the ceramic, observing the surface condition, soaking the ceramic in a sodium hydroxide solution with the concentration of 0.6mol/L at 50 ℃ for 150 hours, taking out, cleaning and drying the ceramic by using the deionized water, weighing the quality of the ceramic again, and comparing the quality with the quality of the ceramic before and after the ceramic is changed.
By conducting the acid resistance test on the ceramics in examples 1 to 11, the surface and quality of the ceramics were not changed before and after the test. By alkali resistance testing of the ceramics of examples 1-11, the surface and quality of the ceramics before and after testing were not changed, and it is seen that the ceramics of the examples of the invention have better corrosion resistance.
From the test results, the ceramic prepared by the method in the embodiment of the invention has the advantages of strong corrosion resistance, high tensile strength, good wear resistance, good durability and stability, and can meet the use requirements.
The foregoing provides some embodiments of the present invention, and the detailed descriptions are provided, so that the scope of the present invention is not limited to the above-mentioned embodiments, and modifications made by those skilled in the art under the common general knowledge or the combination of conventional techniques are also included in the scope of the present invention.
Claims (10)
1. The preparation method of the environment-friendly ceramic is characterized by comprising the following steps:
Step S1, grinding and mixing kaolin, boron oxide, carbon powder, zirconium, barium carbonate, calcium carbonate, boron, silicon and titanium to obtain a mixture;
mixing zinc nitrate, zirconium nitrate and a dispersing agent to obtain a mixed solution;
Mixing the mixture with the mixed solution to obtain mixed slurry;
S2, preparing the mixed slurry into a blank to be sintered;
s3, placing the blank in a sintering furnace, heating to a first temperature of 560-720 ℃ and treating for 1.5-4h in a first treatment environment;
step S4, heating the sintering furnace from the first temperature 560-720 ℃ to the second temperature 880-1130 ℃ and treating for 2-5h in a second treatment environment;
step S5, heating the sintering furnace from the second temperature 880-1130 ℃ to a third temperature 1280-1420 ℃ and treating for 3-6h in a third treatment environment;
step S6, heating the sintering furnace from the third temperature 1280-1420 ℃ to the fourth temperature 1530-1620 ℃ for 1-3h in a fourth treatment environment;
The first processing environment comprises a vacuum or inert atmosphere, the second processing environment comprises a vacuum or inert atmosphere, the third processing environment comprises a vacuum or inert atmosphere, and the fourth processing environment comprises a vacuum or inert atmosphere.
2. The method of manufacturing according to claim 1, wherein the raw materials for manufacturing the ceramic include:
12-25 parts of kaolin;
2.5-4.5 parts by weight of boron oxide;
0.5 to 1.3 parts by weight of carbon powder;
Zirconium 0.7-1.6 weight portions;
0.5 to 1.2 parts by weight of barium carbonate;
0.4-0.9 parts by weight of calcium carbonate;
0.3-0.7 parts by weight of zinc nitrate;
zirconium nitrate 0.6-1.8 weight portions;
0.5 to 1.4 parts by weight of boron;
0.4-0.8 parts by weight of silicon;
Titanium 0.3-1.2 weight portions.
3. The method of claim 1 or 2, wherein the first process environment is a vacuum, the second process environment comprises nitrogen, argon, the third process environment comprises nitrogen, argon, and the fourth process environment is a vacuum.
4. The method according to claim 1 or 2, wherein the third treatment environment comprises nitrogen, argon, silane, methane, boron trichloride, the volume of silane in the third treatment atmosphere is 1.5-4%, the volume of methane in the third treatment atmosphere is 2-5%, the volume of boron trichloride in the third treatment environment is 1-3%, and the volume of nitrogen in the third treatment environment is 8-15%;
the fourth processing environment is a vacuum.
5. The method of claim 1, wherein the kaolin is a modified kaolin, the method of preparing the modified kaolin comprising:
placing kaolin into an acidic solution for pickling;
Placing the kaolin subjected to acid washing in a calcium hydroxide solution for mixing treatment;
Then drying to obtain a dried product;
Then mixing the dried product with boron oxide, aluminum, carbon powder, silicon and tungsten trioxide to obtain a mixture;
Treating the mixture in vacuum at 620-780 ℃ for 0.5-1.5h;
Then the mixture is placed in a treatment gas for 2 to 3.5 hours at 1150 to 1320 ℃;
then cooling and grinding to obtain modified kaolin;
the process gas includes nitrogen and argon.
6. The method according to claim 5, wherein boron oxide in the mixture is 0.5 to 0.9% by mass of kaolin, aluminum in the mixture is 0.3 to 0.7% by mass of kaolin, carbon powder in the mixture is 0.7 to 1.2% by mass of kaolin, silicon in the mixture is 0.5 to 1% by mass of kaolin, and tungsten trioxide in the mixture is 0.3 to 0.8% by mass of kaolin.
7. The method of claim 5, wherein the nitrogen in the process gas is 12-25% by volume.
8. The method according to claim 1 or 5, wherein the raw materials for preparing the ceramic further comprise:
The preparation method of the modified mullite comprises the following steps:
placing mullite in water at 60-85 ℃ for treatment for 1-2h;
filtering and drying to obtain a filtered substance;
then mixing the filter material with titanium boride, zirconium oxide, boron carbide and carbon powder to obtain mixed powder;
Placing the mixed powder in vacuum and treating for 0.5-1h at 950-1160 ℃;
then the mixed powder is placed in modified gas to be treated for 1 to 3 hours at 1220 to 1400 ℃;
Finally, cooling and grinding to obtain modified mullite;
The titanium boride in the mixed powder is 0.5-1% of the mullite, the zirconia in the mixed powder is 0.3-0.8% of the mullite, the boron carbide in the mixed powder is 0.5-1.3% of the mullite, and the carbon powder in the mixed powder is 0.6-1% of the mullite;
the modified gas comprises nitrogen, argon and silane, wherein the volume of the nitrogen in the modified gas is 7-13%, and the volume of the silane in the modified gas is 1.2-2.5%.
9. The method according to claim 8, wherein the modified mullite is contained in an amount of 6 to 11 parts by weight.
10. An environmentally friendly ceramic prepared by the preparation method of any one of claims 1 to 9.
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