CN113956024B - Thermal shock resistant composite ceramic material - Google Patents
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Abstract
The invention relates to a thermal shock resistant composite ceramic material, which specifically comprises the following raw materials of 60-68% by mass of alumina, 15-21% by mass of zirconia and 11-25% by mass of mullite, wherein the sum of the addition amounts of the alumina, the zirconia and the mullite is 100%. Compared with the prior art, the prepared complex phase ceramic material is directly added with alumina with high hardness and high compressive strength, mullite with lower thermal expansion coefficient and zirconia with corrosion resistance and high melting point, has the characteristics of high strength, good thermal shock resistance and the like, and is simple to prepare, easy to operate and low in cost.
Description
Technical Field
The invention relates to a ceramic material, in particular to a thermal shock resistant complex phase ceramic material.
Background
The ceramic material has the characteristics of high hardness, oxidation resistance, corrosion resistance and the like, and is widely applied to various scenes, but the ceramic material is brittle and is easy to break when subjected to thermal shock, so that the application range of the ceramic material is limited.
Alumina (Al) 2 O 3 ) Has various crystalline states, higher melting point (2015 ℃), higher hardness and higher Young modulus; the single-layer alumina ceramic material has the characteristics of good wear resistance, low price, rich resources and the like, and is widely applied, but the single-layer alumina ceramic material has poor thermal shock resistance, and the strength retention rate is only 22% after thermal shock at the temperature difference of 300 ℃.
Chinese patent CN106927840B discloses a thermal shock resistant complex phase ceramic and a preparation method of a ceramic discharge spout based on the same, and the mass fractions of the prepared raw materials are respectively Al 2 O 3 69.01％～76.00％、ZrO 2 17.01％～24.13％、SiO 2 5.29 to 5.97 percent, mgO 0.05 to 0.89 percent or Y 2 O 3 0.05％～1.33％、TiO 2 0.05 to 0.19 percent of binder and 0.5 to 1.5 percent of binder, and sintering the mixture at a high temperature of 1630 to 1680 ℃ after isostatic pressing at 90 to 220MPa to prepare the thermal shock resistant composite ceramic material discharge spout which has the advantages of high temperature resistance, molten metal erosion resistance and thermal shock resistanceExcellent thermal shock property and the like. However, in this patent, the mullite is made of Al 2 O 3 The formed corundum phase matrix phase and the added SiO 2 The ceramic material is prepared by sintering, needs isostatic pressing at 90-220 MPa, is sintered at a high temperature of 1630-1680 ℃, is complex to prepare and has high cost, and the invention does not particularly show the thermal shock resistance of the thermal shock resistant ceramic material.
The alumina-mullite high-temperature composite ceramic modification research (Fanfar, silicate report, no. 4 of 2020) discloses a preparation method of alumina-mullite-zirconia composite ceramic, the mass fractions of the used raw materials are alumina 52%, mullite 26% and zirconia 22%, the method improves the thermal shock resistance of the material by reducing the alumina content and increasing the mullite content, but the prepared material has low mechanical strength (200-205 MPa) and the bulk density of 3.5g/cm 3 Therefore, the strength of the alumina-zirconia-mullite composite ceramic cannot be improved, and the air cooling thermal shock of the ceramic material at 1500-20 ℃ is only improved by 50 percent.
Therefore, extensive attention is paid to research and development of ceramic materials with strong thermal shock resistance and good mechanical properties.
Disclosure of Invention
In order to overcome the defects of the existing ceramic material, the invention provides a thermal shock resistant complex phase ceramic material with high temperature resistance and high strength.
The purpose of the invention can be realized by the following technical scheme:
the invention provides a thermal shock resistant composite ceramic material, which takes alumina as a main crystal phase and zirconia and mullite as a bonding phase, wherein in the thermal shock resistant composite ceramic material, the mass percent of the alumina is 60-68%, the mass percent of the zirconia is 15-21%, the mass percent of the mullite is 11-25%, and the sum of the addition of the alumina, the zirconia and the mullite is 100%.
In one embodiment of the invention, the mullite is fused mullite.
In one embodiment of the invention, in the thermal shock resistant composite ceramic material, the mass percent of alumina is 60%, the mass percent of zirconia is 15%, and the mass percent of mullite is 25%.
In one embodiment of the invention, in the thermal shock resistant composite ceramic material, the mass percent of alumina is 61%, the mass percent of zirconia is 21%, and the mass percent of mullite is 18%.
In one embodiment of the invention, in the thermal shock resistant composite ceramic material, the mass percent of alumina is 65%, the mass percent of zirconia is 18%, and the mass percent of mullite is 17%.
In one embodiment of the invention, in the thermal shock resistant composite ceramic material, the mass percent of alumina is 65%, the mass percent of zirconia is 15%, and the mass percent of mullite is 20%.
In one embodiment of the invention, in the thermal shock resistant composite ceramic material, the mass percent of alumina is 68%, the mass percent of zirconia is 16%, and the mass percent of mullite is 16%.
In one embodiment of the invention, in the thermal shock resistant composite ceramic material, the mass percent of alumina is 68%, the mass percent of zirconia is 15%, and the mass percent of mullite is 17%.
In one embodiment of the invention, the preparation method of the thermal shock resistant complex phase ceramic material comprises the following steps: adding deionized water into alumina, zirconia and mullite, carrying out wet ball milling, drying in a drying oven, sieving, granulating, carrying out dry pressing, sintering, and cooling along with a furnace to obtain the thermal shock resistant composite ceramic material.
In one embodiment of the present invention, the dry press molding conditions are: dry pressing under 30-40 MPa.
In one embodiment of the present invention, the sintering conditions are: and preserving the heat at 1580-1620 ℃ for 1.5-2.5 hours for sintering.
In the prior art, the thermal shock resistance of the material is improved by reducing the content of alumina and increasing the content of mullite. The raw material formula and the preparation process are optimized on the premise of improving the content of the aluminum oxide, the performance of the material is improved, and the method is a technical concept different from the prior art.
According to the thermal shock resistant composite ceramic material, the thermal shock resistance of the composite ceramic can be improved by introducing the zirconia and the mullite into the alumina ceramic material. Zirconium oxide (ZrO) 2 ) The composite material is added into an alumina ceramic material, and the thermal stress generated by thermal shock is relieved through the volume effect caused by phase change, so that the bending strength and the fracture toughness of the composite material are improved. Mullite (2 SiO) 2 ·3Al 2 O 3 ) The composite ceramic has the advantages of high temperature resistance, small heat conductivity coefficient and low thermal expansion coefficient, mullite is introduced into the composite ceramic, and the thermal shock resistance of the composite ceramic is improved by reducing the thermal expansion of the composite ceramic.
According to the thermal shock resistance principle, on the basis of the alumina raw material with high melting point and high hardness, the zirconium oxide with good corrosion resistance and high strength and the mullite with low thermal expansion coefficient are added, so that the obtained finished product only contains three phases which are respectively as follows: the alpha-alumina phase, the zirconia phase and the mullite phase have the characteristics of high compressive strength, high density, good thermal shock resistance and the like.
Compared with the prior art, the invention has the following positive effects:
the mullite added in the application is the fused mullite which is made of Al in comparison with the prior art 2 O 3 The formed corundum phase matrix phase and the added SiO 2 The sintered mullite has improved thermal shock resistance and relatively good high-temperature mechanical property.
According to the application, the optimal formula is obtained by optimizing the raw material formula and the preparation process, so that the thermal shock resistant composite ceramic material has higher density, mechanical strength and thermal shock resistance.
Because the aluminum oxide adopted by the invention has rich resources and low price, the cost of the obtained finished product is low; the raw materials adopted by the invention have few impurity phases, so the purity of the obtained finished product is high; because the raw materials adopted by the invention can improve the thermal shock resistance of the complex phase material, the obtained finished product has high compressive strength and good mechanical property.
Drawings
FIG. 1: example 2X-Ray spectrum and analysis result of thermal shock resistant complex phase ceramic, it can be seen that the obtained complex phase ceramic only contains alpha-alumina phase, zirconia phase and mullite phase;
FIG. 2 is a schematic diagram: in the SEM photograph of the thermal shock resistant composite ceramic powder of example 2, the bright part at 1 point is zirconia, and it can be seen that the integral shape of the particles is complete and the size distribution of the particles are uniform.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
In the following examples, the material performance test methods are illustrated as follows:
(1) And (3) compactness: sample volume measured using archimedes drainage method.
(2) Bending strength: a three-point bending method is adopted, and particularly according to a GB/T6569-2006 fine ceramic bending strength test method.
(3) Thermal shock resistance: according to YB/T376.3-2004, a heating furnace is preheated to 1500 +/-10 ℃, the temperature is kept for 15min, then a sample is quickly inserted into a hearth, the temperature is kept for 20min, the sample is taken out and quickly placed in a place where air flows, the sample is placed in red ink after the test is finished, the red ink is taken out after the test is finished, the red ink is kept still for 30min, whether cracks exist or not is observed, and the breaking strength is tested.
Example 1
The thermal shock resistant complex phase ceramic material blank of the embodiment comprises the following components in percentage by mass: 60% of alumina, 25% of mullite and 15% of zirconia, adding a proper amount of deionized water, carrying out wet ball milling for 5h, then drying for 10h by a drying oven, sieving, granulating, carrying out dry pressing molding under 31MPa, carrying out heat preservation at 1600 ℃ for 2h, sintering, and carrying out furnace cooling to obtain the alumina-based complex phase material. The relevant data are shown in table 1.
Example 2
The mass percentage of the thermal shock resistant complex phase ceramic material blank in the embodiment is as follows: adding an appropriate amount of deionized water into 61% of alumina, 18% of mullite and 21% of zirconia, carrying out wet ball milling for 5 hours, drying for 10 hours in a drying oven, sieving, granulating, carrying out 31MPa dry pressing for molding, carrying out heat preservation at 1600 ℃ for 2 hours, sintering, and carrying out furnace cooling to obtain the alumina-based complex phase material. The relevant data are shown in table 1.
Example 3
The mass percentage of the thermal shock resistant complex phase ceramic material blank in the embodiment is as follows: 65% of alumina, 17% of mullite and 18% of zirconia, adding a proper amount of deionized water, carrying out wet ball milling for 3h, then drying for 10h by a drying oven, sieving, granulating, carrying out 40MPa dry pressing molding, carrying out heat preservation at 1610 ℃ for 2h, sintering, and carrying out furnace cooling to obtain the alumina-based complex phase material. The relevant data are shown in Table 1.
Example 4
The thermal shock resistant complex phase ceramic material blank of the embodiment comprises the following components in percentage by mass: 65% of alumina, 20% of mullite and 15% of zirconia, adding a proper amount of deionized water, carrying out wet ball milling for 5h, drying for 8h in a drying oven, sieving, granulating, carrying out 40MPa dry pressing molding, carrying out heat preservation at 1580 ℃ for 2h, sintering, and carrying out furnace cooling to obtain the alumina-based complex phase material. The relevant data are shown in table 1.
Example 5
The thermal shock resistant complex phase ceramic material blank of the embodiment comprises the following components in percentage by mass: 68% of alumina, 16% of mullite and 16% of zirconia, adding a proper amount of deionized water, carrying out wet ball milling for 2h, drying for 8h in a drying oven, sieving, granulating, carrying out 40MPa dry pressing for molding, carrying out heat preservation at 1620 ℃ for 2h for sintering, and carrying out furnace cooling to obtain the alumina-based complex phase material. The relevant data are shown in Table 1.
Example 6
The thermal shock resistant complex phase ceramic material blank of the embodiment comprises the following components in percentage by mass: 68% of alumina, 17% of mullite and 15% of zirconia, adding a proper amount of deionized water, carrying out wet ball milling for 2h, drying for 8h by a drying oven, sieving, granulating, carrying out dry pressing molding under 31MPa, carrying out heat preservation at 1590 ℃ for 2h, sintering, and carrying out furnace cooling to obtain the alumina-based complex phase material. The relevant data are shown in Table 1.
Comparative example
The mass percentage of the thermal shock resistant complex phase ceramic material blank of the comparative example is as follows: adding a proper amount of deionized water into 52% of alumina, 26% of mullite and 22% of zirconia, carrying out wet ball milling for 2h, then drying for 12h by a drying oven, sieving, granulating, carrying out 16MPa dry pressing for molding, carrying out heat preservation at 1650 ℃ for 2h for sintering, and carrying out furnace cooling to obtain the alumina-based complex phase material. The relevant data are shown in table 1.
TABLE 1 Performance data for the materials obtained in the examples and comparative examples
It can be seen from the results of examples 1 and 2 that the preparation process is the same, the only difference is that the component ratios are different, and the obtained material has larger difference in performance, so that the main influence factor is the raw material ratio. In other embodiments, except for different raw material ratios, the preparation processes are slightly different, such as ball milling time, drying time, pressure and sintering temperature, but are not main influencing factors.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (7)
1. The thermal shock resistant composite ceramic material is characterized in that alumina is used as a main crystalline phase, zirconia and mullite are used as a binding phase, the mass percent of the alumina is 60-68%, the mass percent of the zirconia is 15-21%, the mass percent of the mullite is 11-25%, and the sum of the addition amount of the alumina, the zirconia and the mullite is 100%;
the mullite is fused mullite;
the preparation method of the thermal shock resistant complex phase ceramic material comprises the following steps: adding deionized water into alumina, zirconia and mullite, performing wet ball milling, drying by a drying oven, sieving, granulating, performing dry press molding, sintering, and furnace cooling to obtain the thermal shock resistant composite ceramic material, wherein the dry press molding conditions are as follows: dry pressing and forming under the condition of 30-40MPa, wherein the sintering condition is as follows: preserving heat at 1580-1620 ℃ for 1.5-2.5 hours for sintering;
adding zirconia into an alumina ceramic material, relieving thermal stress generated by thermal shock through a volume effect caused by phase change, improving the bending strength and fracture toughness of the complex phase material, introducing mullite into the complex phase ceramic, and improving the thermal shock resistance of the complex phase ceramic by reducing the thermal expansion property of the complex phase ceramic; the thermal shock resistant complex phase ceramic material only contains three phases which are respectively as follows: an alpha-alumina phase, a zirconia phase, and a mullite phase.
2. The thermal shock resistant composite ceramic material according to claim 1, wherein in the thermal shock resistant composite ceramic material, the mass percent of alumina is 60%, the mass percent of zirconia is 15%, and the mass percent of mullite is 25%.
3. The thermal shock resistant composite ceramic material according to claim 1, wherein the thermal shock resistant composite ceramic material comprises 61 mass percent of alumina, 21 mass percent of zirconia and 18 mass percent of mullite.
4. The thermal shock resistant composite ceramic material as claimed in claim 1, wherein the thermal shock resistant composite ceramic material comprises 65 mass percent of alumina, 18 mass percent of zirconia and 17 mass percent of mullite.
5. The thermal shock resistant composite ceramic material as claimed in claim 1, wherein the thermal shock resistant composite ceramic material comprises 65 mass percent of alumina, 15 mass percent of zirconia and 20 mass percent of mullite.
6. The thermal shock resistant composite ceramic material according to claim 1, wherein in the thermal shock resistant composite ceramic material, the mass percent of alumina is 68%, the mass percent of zirconia is 16%, and the mass percent of mullite is 16%.
7. The thermal shock resistant composite ceramic material as claimed in claim 1, wherein the thermal shock resistant composite ceramic material comprises 68 mass percent of alumina, 15 mass percent of zirconia and 17 mass percent of mullite.
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