CN111592341B - Preparation method of porous alumina ceramic - Google Patents
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Abstract
A preparation method of porous alumina ceramics belongs to the technical field of structural ceramic materials. The invention aims to solve the matching problem of thermal shock damage resistance and thermal shock fracture resistance of the existing alumina ceramic material. The invention uses a gel injection molding method in combination with a pore-forming agent adding method, changes the microstructure of the material by controlling the content of the pore-forming agent, prepares the porous alumina ceramic with the porosity of 24.42-41.10% under the condition of pressureless sintering at 1600 ℃, has the variation range of thermal conductivity of 10.354-14.018W/(m.K), the critical temperature difference range of 320-386 ℃, has the retention rate of residual strength of more than 40% when being subjected to thermal shock by the temperature difference of 500 ℃, has good thermal shock resistance, and obtains the porous alumina ceramic material with high thermal shock fracture resistance and high thermal shock damage resistance when the volume fraction of the pore-forming agent dosage alumina powder is 30%.
Description
Technical Field
The invention relates to a preparation method of porous alumina ceramic, belonging to the technical field of structural ceramic materials.
Background
The alumina ceramic has good high temperature resistance, good thermal conductivity, high mechanical strength and good electromechanical property, and is widely applied to a plurality of fields such as machinery, purification and separation, sound absorption and shock absorption, chemical catalytic carriers, sensor materials and the like. Alumina-based ceramic cores made from alumina ceramic materials are becoming more and more widely used under high temperature and pressure conditions.
The thermal shock damage resistance of the alumina ceramic material prepared by the existing method is increased along with the increase of the porosity of a sample, and the thermal shock fracture resistance is reduced along with the increase of the porosity, so that the porosity and the strength can not be considered at the same time, and the application of the alumina ceramic material is limited. Therefore, it is necessary to provide a preparation method of porous alumina ceramic to solve the matching problem of thermal shock damage resistance and thermal shock fracture resistance of the existing alumina ceramic material.
Disclosure of Invention
The invention provides a preparation method of porous alumina ceramic, aiming at solving the problem of matching thermal shock damage resistance and thermal shock fracture resistance of the existing alumina ceramic material.
The technical scheme of the invention is as follows:
the preparation method of the porous alumina ceramic comprises the following specific operation steps:
step one, preparing slurry: uniformly mixing alumina powder, magnesia, agarose and a ceramic pore-forming agent, and ball-milling for 4-6 hours by using deionized water as a medium and using an alumina milling ball to obtain slurry;
step two, injection molding: heating the slurry obtained in the step one to 80-97 ℃, injecting the slurry into a mold, and naturally cooling the slurry to room temperature to obtain a molded sample;
step three, removing glue: putting the molded sample obtained in the step two into a high-temperature resistance furnace, heating the molded sample to 600 ℃ from room temperature, and preserving the heat for 1 hour;
Step four, sintering: and (3) carrying out pressureless sintering on the molded sample subjected to the glue discharge in the step three, wherein the sintering conditions are as follows: the room temperature is heated to 1600 ℃ at the heating rate of 3 ℃/min-5 ℃/min, the temperature is kept for 2 hours, and the porous alumina ceramic is obtained after furnace cooling.
The mass ratio of the alumina powder to the magnesia to the agarose is 1: 0.01: 0.01.
the addition amount of the ceramic pore-forming agent is 10-50% of the volume of the alumina powder.
The addition amount of the ceramic pore-forming agent is 20 percent, 30 percent and 40 percent of the volume of the alumina powder.
The volume ratio of the deionized water to the alumina powder is 2: 3.
The ball milling time in the step one is 5 hours.
In the second step, the slurry is heated to 85 ℃.
The porosity of the porous alumina ceramic is 24.42-41.10%, the heat conductivity coefficient is 10.354-14.018W/(m.K), the bending strength is 88-116 Mpa, and the critical temperature difference is 320-386 ℃.
The invention has the following beneficial effects: the invention relates to a preparation method of porous alumina ceramic, which adopts a gel casting combined with a pore-forming agent adding method to prepare the porous alumina ceramic with the porosity of 24-40%, the variation range of the thermal conductivity coefficient is 10.354-14.018W/(m.K), the critical temperature difference range is 320-386 ℃, the retention rate of the residual strength is more than 40% when the ceramic is subjected to thermal shock by the temperature difference of 500 ℃, the ceramic has good thermal shock resistance, and the problem of matching the thermal shock damage resistance and the thermal shock fracture resistance of the existing ceramic material is solved. And when the volume fraction of the pore-forming agent is 30 percent of that of the alumina powder, the porous alumina ceramic material with high thermal shock fracture resistance and high thermal shock damage resistance is obtained. In addition, the porous alumina ceramic prepared by the method has the advantages of environment-friendly and non-toxic component composition, low cost, high heat conductivity and the like.
Drawings
FIG. 1 is an SEM image of porous alumina ceramic prepared by the method of the present invention.
Detailed Description
The experimental procedures used in the following examples are conventional unless otherwise specified.
The alumina powders referred to in the following specific examples are commercially available micron-sized alpha-Al2O3Purity not less than 99.5%, d500.2 μm; the ceramic pore-forming agent is PL-100, manufactured by Baolimei plastics Co., Ltd, Dongguan.
Embodiment mode 1: the addition amount of the ceramic pore-forming agent is 10 percent of the volume of the alumina powder
131.67g of alumina powder is added with 1.32g of magnesia, 1.32g of agarose and 4g of ceramic pore-forming agent, 50ml of deionized water is taken as a medium, and after uniform mixing, 150g of alumina grinding balls are added for ball milling for 5 hours at the rotation speed of 1200rpm, thus obtaining slurry. And then heating the slurry to 85 ℃, injecting the heated slurry into a mold, naturally cooling the heated slurry to room temperature, and drying the cooled slurry to obtain a cylindrical molding sample with the diameter of 35 mm. The sample was placed in an electric resistance furnace and heated from room temperature to 600 ℃ for 20 hours, and then taken out after 1 hour of heat preservation. Then putting the mixture into a high-temperature resistance sintering furnace for pressureless sintering, wherein the sintering conditions are as follows: the room temperature is heated to 1600 ℃ at the heating rate of 5 ℃/min, the temperature is kept for 2 hours, and the porous alumina ceramic is obtained after furnace cooling.
And (3) testing the performance of the porous alumina ceramic: the porous alumina ceramic obtained by sintering was cut, ground and polished to obtain a 3mm × 4mm × 35mm test strip.
The above test strip was boiled for 2 hours and then measured to have a density of 2.99g/cm by a drainage method3。
The bending strength of the sample is measured to be 116.4MPa by using a three-point bending method (span of 30mm) by using a national standard GB/T6569-2006 fine ceramic bending strength test method.
After thermal shock at 500 ℃ in temperature difference, the retention rate of residual strength reaches 45.77%, and the critical temperature difference is 367 ℃.
The thermal conductivity of the sample was 14.02W/(mK) by the laser pulse method.
Embodiment mode 2: the addition amount of the ceramic pore-forming agent is 20 percent of the volume of the alumina powder
131.67g of alumina powder is added with 1.32g of magnesia, 1.32g of agarose and 8g of ceramic pore-forming agent, 50ml of deionized water is taken as a medium, and after uniform mixing, 150g of alumina grinding balls are added to carry out ball milling for 5 hours at the rotating speed of 1200rpm, thus obtaining slurry. And then heating the slurry to 85 ℃, injecting the heated slurry into a mold, naturally cooling the heated slurry to room temperature, and drying the cooled slurry to obtain a cylindrical molding sample with the diameter of 35 mm. The sample was placed in an electric resistance furnace and heated from room temperature to 600 ℃ for 20 hours, and then taken out after 1 hour of heat preservation. Then putting the mixture into a high-temperature resistance sintering furnace for pressureless sintering, wherein the sintering conditions are as follows: the room temperature is heated to 1600 ℃ at the heating rate of 5 ℃/min, the temperature is kept for 2 hours, and the porous alumina ceramic is obtained after furnace cooling.
And (3) testing the performance of the porous alumina ceramic: the porous alumina ceramic obtained by sintering was cut, ground and polished to obtain a 3mm × 4mm × 35mm test strip.
The above test bar was boiled for 2 hours and then measured to have a density of 2.84g/cm by a drainage method3。
The bending strength of the sample is 107.5MPa measured by a three-point bending method (span of 30mm) by using a national standard GB/T6569-2006 fine ceramic bending strength test method.
After thermal shock by the temperature difference of 500 ℃, the retention rate of the residual strength reaches 45.80%, and the critical temperature difference is 373 ℃.
The thermal conductivity of the sample was measured by the laser pulse method to be 13.06W/(m.K).
Embodiment mode 3: the addition amount of the ceramic pore-forming agent is 30 percent of the volume of the alumina powder
131.67g of alumina powder is added with 1.32g of magnesia, 1.32g of agarose and 12g of ceramic pore-forming agent, 50ml of deionized water is taken as a medium, and after uniform mixing, 150g of alumina grinding balls are added to carry out ball milling for 5 hours at the rotating speed of 1200rpm, thus obtaining slurry. And then heating the slurry to 85 ℃, injecting the heated slurry into a mold, naturally cooling the heated slurry to room temperature, and drying the cooled slurry to obtain a cylindrical molding sample with the diameter of 35 mm. The sample was placed in an electric resistance furnace and heated from room temperature to 600 ℃ for 20 hours, and then taken out after 1 hour of heat preservation. Then putting the mixture into a high-temperature resistance sintering furnace for pressureless sintering, wherein the sintering conditions are as follows: the room temperature is heated to 1600 ℃ at the heating rate of 5 ℃/min, the temperature is kept for 2 hours, and the porous alumina ceramic is obtained after furnace cooling.
And (3) testing the performance of the porous alumina ceramic: the porous alumina ceramic obtained by sintering was cut, ground and polished to obtain a 3mm × 4mm × 35mm test strip.
The above test strip was boiled for 2 hours and then measured to have a density of 2.63g/cm by a drainage method3。
The bending strength of the sample is measured to be 98.38MPa by using a three-point bending method (span of 30mm) by using a national standard GB/T6569-2006 fine ceramic bending strength test method.
After thermal shock by the temperature difference of 500 ℃, the retention rate of the residual strength reaches 47.28%, and the critical temperature difference is 386 ℃.
The thermal conductivity of the sample was measured by the laser pulse method to be 12.16W/(mK).
Embodiment 4: the addition amount of the ceramic pore-forming agent is 40 percent of the volume of the alumina powder
131.67g of alumina powder is added with 1.32g of magnesia, 1.32g of agarose and 16g of ceramic pore-forming agent, 50ml of deionized water is taken as a medium, and after uniform mixing, 150g of alumina grinding balls are added to carry out ball milling for 5 hours at the rotating speed of 1200rpm, thus obtaining slurry. And then heating the slurry to 85 ℃, injecting the heated slurry into a mold, naturally cooling the heated slurry to room temperature, and drying the cooled slurry to obtain a cylindrical molding sample with the diameter of 35 mm. The sample was placed in an electric resistance furnace and heated from room temperature to 600 ℃ for 20 hours, and then taken out after 1 hour of heat preservation. Then putting the mixture into a high-temperature resistance sintering furnace for pressureless sintering, wherein the sintering conditions are as follows: the room temperature is heated to 1600 ℃ at the heating rate of 5 ℃/min, the temperature is kept for 2 hours, and the porous alumina ceramic is obtained after furnace cooling.
And (3) testing the performance of the porous alumina ceramic: the porous alumina ceramic obtained by sintering was cut, ground and polished to obtain a 3mm × 4mm × 35mm test strip.
The above test bar was boiled for 2 hours and then measured to have a density of 2.44g/cm by a drainage method3。
The bending strength of the sample is 93.14MPa measured by a three-point bending method (span of 30mm) by using a national standard GB/T6569-2006 fine ceramic bending strength test method.
After thermal shock by 500 ℃ temperature difference, the residual strength retention rate reaches 42.94%, and the critical temperature difference is 350 ℃.
The thermal conductivity of the sample was 10.95W/(mK) by the laser pulse method.
Embodiment 5: the addition amount of the ceramic pore-forming agent is 50 percent of the volume of the alumina powder
131.67g of alumina powder is added with 1.32g of magnesia, 1.32g of agarose and 20g of ceramic pore-forming agent, 50ml of deionized water is taken as a medium, and after uniform mixing, 150g of alumina grinding balls are added to carry out ball milling for 5 hours at the rotating speed of 1200rpm, thus obtaining slurry. And then heating the slurry to 85 ℃, injecting the heated slurry into a mold, naturally cooling the heated slurry to room temperature, and drying the cooled slurry to obtain a cylindrical molding sample with the diameter of 35 mm. The sample was placed in an electric resistance furnace and heated from room temperature to 600 ℃ for 20 hours, and then taken out after 1 hour of heat preservation. Then putting the mixture into a high-temperature resistance sintering furnace for pressureless sintering, wherein the sintering conditions are as follows: the room temperature is heated to 1600 ℃ at the heating rate of 5 ℃/min, the temperature is kept for 2 hours, and the porous alumina ceramic is obtained after furnace cooling.
And (3) testing the performance of the porous alumina ceramic: the porous alumina ceramic obtained by sintering was cut, ground and polished to obtain a 3mm × 4mm × 35mm test strip.
The above test bar was boiled for 2 hours and then measured to have a density of 2.33g/cm by a drainage method3。
The bending strength of the sample is 88.68MPa measured by using a three-point bending method (span of 30mm) of a national standard GB/T6569-2006 fine ceramic bending strength test method.
After thermal shock by 500 ℃ temperature difference, the residual strength retention rate reaches 44.23%, and the critical temperature difference is 320 ℃.
The thermal conductivity of the sample was 10.35W/(mK) by the laser pulse method.
The performance pairs of the porous alumina ceramic material prepared by different ceramic pore-forming agent addition amounts are as follows:
from the above table, the thermal conductivity of the porous alumina ceramic decreases with the increase of the total porosity, and the critical temperature difference of the material shows a trend of decreasing after a small increase. The residual strength retention rate of the material after being subjected to thermal shock of 500 ℃ temperature difference is in a trend of increasing and then decreasing along with the increase of the total porosity, and different from the trend that the thermal shock fracture resistance is reduced along with the increase of the porosity and the thermal shock damage resistance is increased along with the increase of the porosity in the research of other scholars, the porous alumina ceramic material with high thermal shock fracture resistance and high thermal shock damage resistance is obtained when the using amount of the pore-forming agent is 30 vol%.
The critical temperature difference is the temperature difference corresponding to the ratio of the residual strength to the initial strength of the material after thermal shock of 70%. The greater the critical temperature difference of the material, the better the thermal shock fracture resistance of the material. The critical temperature differences for 24.42%, 28.01%, 33.45%, 38.17% and 41.10% porosity were 367 ℃, 373 ℃, 386 ℃, 350 ℃ and 320 ℃, respectively. The porosity increases and then decreases. Unlike the theoretical critical temperature difference which decreases with increasing porosity, according to the relationship between the ultimate strength of the material and the critical temperature difference:wherein R' is referred to as a second thermal stress rupture resistance factor; sigmafIs the ultimate strength of the material. It can be seen that the critical temperature difference is in direct proportion to the ultimate strength and thermal conductivity of the material and in inverse proportion to the elastic modulus. The coefficient of thermal expansion α is substantially invariant with changes in porosity, and the Poisson's ratio μ is roughly considered invariant, as willGiven the constant a, substituting a numerical value, the results of R' for different porosities are as follows: 21.82a, 23.19a, 23.73a, 22.41a and 21.46 a. And R is large, the thermal shock fracture resistance of the material is good. This is consistent with the experimental results showing that the thermal shock fracture resistance of the material is best at a porosity of 33.45%.
The residual strength retention, which represents the ratio of the strength of the ceramic material after being subjected to a thermal shock to the initial strength of the ceramic material, can be used to characterize the thermal shock damage resistance of the material. The residual strength retention for 24.42%, 28.01%, 33.45%, 38.17% and 41.10% porosity at 500 ℃ thermal shock temperature difference was 45.77%, 45.80%, 47.28%, 42.94% and 44.23%, respectively. The fracture surface energies were 21.59, 22.53, 23.57, 23.11 and 22.84J/m, respectively. The fracture surface energy is proportional to the thermal shock damage resistance of the material, and is consistent with the experimental result, which shows that the thermal shock damage resistance of the material shows a trend of increasing and then decreasing.
Claims (4)
1. A preparation method of porous alumina ceramics is characterized in that: the method comprises the following operation processes:
step one, preparing slurry: uniformly mixing alumina powder, magnesia, agarose and a ceramic pore-forming agent, and ball-milling for 4-6 hours by using alumina grinding balls with deionized water as a medium to obtain slurry;
step two, injection molding: heating the slurry obtained in the step one to 80-97 ℃, injecting the slurry into a mold, and naturally cooling the slurry to room temperature to obtain a molded sample;
step three, removing glue: putting the molded sample obtained in the step two into a high-temperature resistance furnace, heating to 600 ℃ at room temperature at the heating rate of 0.5 ℃/min, and preserving heat for 1-2 hours;
Step four, sintering: and (3) carrying out pressureless sintering on the molded sample subjected to the glue discharge in the step three, wherein the sintering conditions are as follows: heating the room temperature to 1600 ℃ at the heating rate of 3-5 ℃/min, preserving the heat for 2 hours, and cooling along with the furnace to obtain porous alumina ceramic;
the mass ratio of the alumina powder to the magnesia to the agarose is 1:0.01: 0.01;
the addition amount of the ceramic pore-forming agent is 30 percent of the volume of the alumina powder.
2. The method of claim 1, wherein the porous alumina ceramic is prepared by: the volume ratio of the deionized water to the alumina powder is 2: 3.
3. The method of claim 1, wherein the porous alumina ceramic is prepared by: the ball milling time in the step one is 5 hours.
4. The method of claim 1, wherein the porous alumina ceramic is prepared by: in the second step, the slurry is heated to 85 ℃.
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