CN113185277A - High-thermal-stability ceramic material and preparation method and application thereof - Google Patents
High-thermal-stability ceramic material and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a high-thermal-stability ceramic material and a preparation method and application thereof, belonging to the technical field of high-entropy ceramic materials. The invention is based on the entropy stabilization effect of high-entropy ceramics, namely LaMgAl11O19The introduction of heavy rare earth elements (Tb, Dy, Ho and Er) with large La radius difference can further increase the lattice distortion degree, further improve the entropy value of the system on the basis of obtaining the maximum configuration entropy by realizing the high entropy change of the ceramic, and maximize the thermal stability of the system, thereby obtaining the ceramic material with high thermal stability. According to the invention, sintering is carried out in a mode of two-stage temperature rise, gradually reduced temperature rise rate of each stage and two-stage temperature reduction, gradually increased temperature reduction rate of each stage, so that the prepared ceramic material has pure phase, and the phase structure is still stable after long-time heat treatment at high temperature without second phaseThe surface has no microcrack, and the method has good application prospect.
Description
Technical Field
The invention relates to the technical field of ceramic materials, in particular to a high-thermal-stability ceramic material and a preparation method and application thereof.
Background
LaMgAl11O19The ceramic has the characteristics of high melting point, small density, low thermal conductivity, large thermal expansion coefficient, large fracture toughness and the like, so the ceramic has wide application space in the fields of heat protection of aerospace vehicles and industrial kilns. However, LaMgAl11O19The thermal stability is reduced at high temperature, and LaAlO is partially decomposed and generated3And thus it is difficult to operate in a high temperature environment for a long time, which severely limits LaMgAl11O19Application and popularization in the fields.
Disclosure of Invention
The invention aims to provide a high-thermal-stability ceramic material, and a preparation method and application thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a high-thermal stability ceramic material, the chemical composition of which is (La)0.4-xTbxDy0.2Ho0.2Er0.2)MgAl11O19Wherein, 0<x≤0.2。
Preferably, x is 0.1 to 0.15.
The invention provides a preparation method of a high-thermal-stability ceramic material, which comprises the following steps:
mixing a lanthanum source, a terbium source, a dysprosium source, a holmium source, an erbium source, a magnesium source and an aluminum source, and performing cold press molding to obtain a blank body; the molar ratio of lanthanum element, terbium element, dysprosium element, holmium element, magnesium element and aluminum element in the lanthanum source, terbium source, dysprosium source, holmium source, erbium element and aluminum source is (0.4-x) x is 0.2:0.2:0.2:1:11, and x is more than 0 and less than or equal to 0.2;
carrying out staged heat preservation on the blank to obtain a high-thermal-stability ceramic material;
the staged heat preservation process comprises the following steps: the first stage is as follows: the calcination temperature is 1400-1450 ℃, and the heat preservation time is 2-3 h; and a second stage: the calcining temperature is 1700-1750 ℃, and the heat preservation time is 4-5 h; and a third stage: the calcination temperature is 1450-1500 ℃, and the heat preservation time is 1-2 h; a fourth stage: the calcination temperature is 1250-1300 ℃, and the heat preservation time is 0.5-1 h.
Preferably, the lanthanum source comprises lanthanum oxide; the terbium source comprises terbium oxide; the dysprosium source comprises dysprosium oxide and the holmium source comprises holmium oxide; the erbium source comprises erbium oxide, the magnesium source comprises magnesium oxide, and the aluminum source comprises aluminum oxide.
Preferably, the particle sizes of the lanthanum source, the neodymium source, the gadolinium source, the samarium source, the rare earth oxide, the magnesium source and the aluminum source are independently 2-10 nm, and the purity is independently more than or equal to 99.9%.
Preferably, the pressure of the cold press molding is 1-2 MPa, and the pressure maintaining time is 2-4 min.
Preferably, the temperature rising rate from the room temperature to the calcination temperature in the first stage is 8-10 ℃/min.
Preferably, the heating rate of the temperature from the calcination temperature of the first stage to the calcination temperature of the second stage is 5-6 ℃/min.
Preferably, the rate of reducing the temperature from the calcination temperature of the second stage to the calcination temperature of the third stage is 2-4 ℃/min; and the rate of reducing the temperature from the calcining temperature of the third stage to the calcining temperature of the fourth stage is 5-8 ℃/min.
The invention provides an application of the high-stability ceramic material in the technical scheme or the high-thermal-stability ceramic material prepared by the preparation method in the technical scheme in the field of thermal protection of aerospace vehicles or the field of industrial kilns.
The invention provides a high-thermal stability ceramic material, the chemical composition of which is (La)0.4-xTbxDy0.2Ho0.2Er0.2)MgAl11O19Wherein, 0<x is less than or equal to 0.2. The invention is based on the entropy stabilization effect of high-entropy ceramics, namely LaMgAl11O19The introduction of heavy rare earth elements (Tb, Dy, Ho and Er) with large La radius difference can further increase the lattice distortion degree, so that the entropy value of the system is increased, and the LaMgAl is realized11O19Ceramic materialOn the basis of high entropy and maximum configuration entropy, the entropy value of the system is further improved, the thermal stability of the system is maximized, and therefore the high-thermal-stability ceramic material is obtained.
The invention provides a preparation method of the ceramic material with high thermal stability, the invention adopts a staged heat preservation process, and sintering is carried out in a mode of two-stage temperature rise, gradually reduced temperature rise rate of each stage, two-stage temperature reduction and gradually increased temperature reduction rate of each stage, so that the prepared ceramic material has pure phase, and the phase structure is still stable after long-time heat treatment at high temperature, no second phase is generated, no microcrack is generated on the surface, and the ceramic material has good application prospect.
Drawings
FIG. 1 is (La) prepared in example 10.2Tb0.2Dy0.2Ho0.2Er0.2)MgAl11O19XRD patterns before and after ceramic heat treatment;
FIG. 2 is (La) prepared in example 10.2Tb0.2Dy0.2Ho0.2Er0.2)MgAl11O19SEM pictures of ceramics;
FIG. 3 shows LaMgAl prepared in comparative example 111O19XRD patterns before and after ceramic heat treatment;
FIG. 4 is (La) prepared in example 20.3Tb0.1Dy0.2Ho0.2Er0.2)MgAl11O19XRD patterns before and after ceramic heat treatment;
FIG. 5 is (La) prepared in example 20.3Tb0.1Dy0.2Ho0.2Er0.2)MgAl11O19SEM pictures of ceramics;
FIG. 6 shows LaMgAl prepared in comparative example 211O19XRD patterns before and after ceramic heat treatment.
Detailed Description
The invention provides a high-thermal stability ceramic material, the chemical composition of which is (La)0.4-xTbxDy0.2Ho0.2Er0.2)MgAl11O19Wherein, 0<x≤0.2。
In the present invention, x is preferably 0.1 to 0.15.
The invention provides a preparation method of a high-thermal-stability ceramic material, which comprises the following steps:
mixing a lanthanum source, a terbium source, a dysprosium source, a holmium source, an erbium source, a magnesium source and an aluminum source, and performing cold press molding to obtain a blank body; the molar ratio of lanthanum element, terbium element, dysprosium element, holmium element, magnesium element and aluminum element in the lanthanum source, terbium source, dysprosium source, holmium source, erbium element and aluminum source is (0.4-x) x is 0.2:0.2:0.2:1:11, and x is more than 0 and less than or equal to 0.2;
carrying out staged heat preservation on the blank to obtain a high-thermal-stability ceramic material;
the staged heat preservation process comprises the following steps: the first stage is as follows: the calcination temperature is 1400-1450 ℃, and the heat preservation time is 2-3 h; and a second stage: the calcining temperature is 1700-1750 ℃, and the heat preservation time is 4-5 h; and a third stage: the calcination temperature is 1450-1500 ℃, and the heat preservation time is 1-2 h; a fourth stage: the calcination temperature is 1250-1300 ℃, and the heat preservation time is 0.5-1 h.
In the present invention, unless otherwise specified, all the starting materials required for the preparation are commercially available products well known to those skilled in the art.
The method comprises the steps of mixing a lanthanum source, a terbium source, a dysprosium source, a holmium source, an erbium source, a magnesium source and an aluminum source, and carrying out cold press molding to obtain a blank. In the present invention, the lanthanum source preferably comprises lanthanum oxide (La)2O3) (ii) a The terbium source preferably comprises terbium (Tb) oxide4O7) (ii) a The dysprosium source preferably comprises dysprosium oxide (Dy)2O3) The holmium source preferably comprises holmium oxide (Ho)2O3) (ii) a The erbium source preferably comprises erbium oxide (Er)2O3) Preferably, the magnesium source comprises magnesium oxide and the aluminum source comprises aluminum oxide.
In the invention, the molar ratio of lanthanum element, terbium element, dysprosium element, holmium element, magnesium element and aluminum element in the lanthanum source, terbium source, dysprosium source, holmium element, magnesium element and aluminum source is (0.4-x) x is 0.2:0.2:0.2:1:11, x is less than or equal to 0.2, and the molar ratio is more preferably 0.2:0.2:0.2:0.2:0.2:1: 11.
In the invention, the lanthanum source, the terbium source, the dysprosium source, the holmium source, the erbium source, the magnesium source and the aluminum source are all in powder form; the particle sizes of the lanthanum source, the terbium source, the dysprosium source, the holmium source, the erbium source, the magnesium source and the aluminum source are preferably and independently 2-10 nm, more preferably 3-6 nm, and the purity is preferably and independently more than or equal to 99.9%.
In the invention, the lanthanum source, the terbium source, the dysprosium source, the holmium source, the erbium source, the magnesium source and the aluminum source are preferably mixed by wet ball milling, and a medium used for the wet ball milling is preferably absolute ethyl alcohol; the ball milling speed is preferably 280-300 rpm, and the ball milling time is preferably 10-12 h. The amount of the absolute ethyl alcohol is not particularly limited in the present invention, and the ball milling can be smoothly performed according to the amount well known in the art.
In the present invention, the cold press forming is preferably performed in a stainless steel mold, which is not particularly limited in the present invention and may be a mold well known in the art; the pressure of the cold press molding is preferably 1-2 MPa, and more preferably 1.5 MPa; the dwell time is preferably 2-4 min, and more preferably 3 min.
The diameter and the shape of the blank are not particularly limited, and the blank is prepared according to the diameter and the shape well known in the field; in an embodiment of the invention, the blank has a diameter of 12mm and is cylindrical in shape.
After the green body is obtained, the invention carries out heat preservation on the green body by stages to obtain the ceramic material with high thermal stability. In the present invention, the staged incubation process comprises: the first stage is as follows: the calcination temperature is 1400-1450 ℃, and the heat preservation time is 2-3 h; and a second stage: the calcining temperature is 1700-1750 ℃, and the heat preservation time is 4-5 h; and a third stage: the calcination temperature is 1450-1500 ℃, and the heat preservation time is 1-2 h; a fourth stage: the calcination temperature is 1250-1300 ℃, and the heat preservation time is 0.5-1 h; the calcination temperature in the first stage is preferably 1420-1440 ℃, and the heat preservation time is preferably 2.2-2.6 h; the calcination temperature of the second stage is preferably 1720-1730 ℃, and the heat preservation time is preferably 4.2-4.4 h; the calcining temperature in the third stage is preferably 1470-1480 ℃, and the heat preservation time is preferably 1.3-1.8 h; the calcination temperature in the fourth stage is preferably 1260-1280 ℃, and the heat preservation time is preferably 0.6-0.8 h. In the invention, the heating rate of the temperature from room temperature to the calcination temperature of the first stage is preferably 8-10 ℃/min, and more preferably 9 ℃/min; the heating rate of heating from the calcination temperature of the first stage to the calcination temperature of the second stage is preferably 5-6 ℃/min, and more preferably 5.5 ℃/min; the rate of cooling from the calcination temperature of the second stage to the calcination temperature of the third stage is preferably 2-4 ℃/min, and more preferably 3 ℃/min; the temperature rise rate of the temperature reduction from the calcination temperature of the third stage to the calcination temperature of the fourth stage is preferably 5-8 ℃/min, and more preferably 6-7 ℃/min.
In the temperature rise stage, the temperature rise rate is slowed down along with the temperature rise, which is beneficial to reducing the internal temperature gradient of the sample, so that the phase structure is single-phase, the internal structure of the material is uniform, and the mutual reaction among different substances can not occur at high temperature. If multiple phases exist within the material, they may react with each other at high temperatures, causing a volume change that may cause the material to fail, especially in the case of materials applied as coatings, which may cause a mismatch between the coating material and the substrate material. In the cooling stage, because the calcining temperature is higher, in order to avoid the stability from being damaged due to thermal stress aggregation caused by over-high cooling speed during furnace cooling, the invention adopts a staged cooling process, the temperature is kept when the temperature is reduced to a certain value, so that the temperature inside the sample is uniformly distributed, the temperature gradient is reduced, and then the temperature is continuously reduced, and the cooling rate is firstly slow and then fast, thereby being beneficial to reducing the thermal stress aggregation inside the sample during cooling and improving the thermal stability of the ceramic material.
In the present invention, the staged incubation is preferably performed in a muffle furnace; the muffle furnace is not particularly limited, and the temperature can be satisfied.
After the staged heat preservation is finished, the obtained material is preferably cooled along with the furnace to obtain the high-thermal-stability ceramic material. The furnace cooling process is not particularly limited in the present invention and may be performed according to a process well known in the art.
The invention provides an application of the high-thermal-stability ceramic material in the technical scheme or the high-thermal-stability ceramic material prepared by the preparation method in the technical scheme in the field of thermal protection of aerospace vehicles or the field of industrial kilns. The method of the present invention is not particularly limited, and the method may be applied according to a method known in the art.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
La2O3Powder (average particle diameter of 10nm, purity greater than or equal to 99.9%) and Tb4O7Powder (average particle diameter of 10nm, purity not less than 99.9%) and Dy2O3Powder (average particle diameter of 10nm, purity of more than or equal to 99.9%) and Ho2O3Powder (average grain diameter of 10nm, purity more than or equal to 99.9 percent) Er2O3Powder (average particle diameter of 10nm, purity greater than or equal to 99.9%) and Al2O3Powder (average particle diameter of 10nm, purity greater than or equal to 99.9%) and MgO powder (average particle diameter of 10nm, purity greater than or equal to 99.9%) as (La)0.2Tb0.2Dy0.2Ho0.2Er0.2)MgAl11O19Is dosed in a stoichiometric ratio of (a), wherein La2O3Powder, Tb4O7Powder and Dy2O3Powder, Ho2O3Powder and Er2O3Powder of Al2O3Mixing the obtained mixture with absolute ethyl alcohol, and carrying out wet ball milling at the ball milling rotation speed of 300rpm for 10 hours to obtain light gray mixed powder, wherein the molar ratio of the powder to the MgO powder is 0.2:0.1:0.2:0.2:0.2:11: 2;
putting the light gray mixed powder into a stainless steel mold, and maintaining the pressure for 2min under the pressure of 2MPa to obtain a cylindrical blank with the diameter of 12 mm;
placing the cylindrical blank into a muffle furnace to obtain a blank with the thickness of 1Heating to 1450 deg.C at a rate of 0 deg.C/min, maintaining for 2h, heating to 1700 deg.C at a rate of 5 deg.C/min, maintaining for 5h, cooling to 1450 deg.C at a rate of 4 deg.C/min, maintaining for 2h, cooling to 1250 deg.C at a rate of 8 deg.C/min, maintaining for 1h, and furnace cooling to obtain (La)0.2Tb0.2Dy0.2Ho0.2Er0.2)MgAl11O19A ceramic material.
Example 2
La2O3Powder (average particle diameter of 10nm, purity greater than or equal to 99.9%) and Tb4O7Powder (average particle diameter of 10nm, purity not less than 99.9%) and Dy2O3Powder (average particle diameter of 10nm, purity of more than or equal to 99.9%) and Ho2O3Powder (average grain diameter of 10nm, purity more than or equal to 99.9 percent) Er2O3Powder (average particle diameter of 10nm, purity greater than or equal to 99.9%) and Al2O3Powder (average particle diameter of 10nm, purity greater than or equal to 99.9%) and MgO powder (average particle diameter of 10nm, purity greater than or equal to 99.9%) as (La)0.3Tb0.1Dy0.2Ho0.2Er0.2)MgAl11O19Is dosed in a stoichiometric ratio of (a), wherein La2O3Powder, Tb4O7Powder and Dy2O3Powder, Ho2O3Powder and Er2O3Powder of Al2O3Mixing the obtained mixture with absolute ethyl alcohol, and carrying out wet ball milling, wherein the molar ratio of the powder to the MgO powder is 0.3:0.05:0.2:0.2:0.2:11:2, the ball milling rotation speed is 280rpm, and the ball milling time is 12 hours, so as to obtain light gray mixed powder;
putting the light gray mixed powder into a stainless steel mold, and maintaining the pressure for 4min under the pressure of 1MPa to obtain a cylindrical blank with the diameter of 12 mm;
putting the cylindrical blank into a muffle furnace, heating to 1400 ℃ at the speed of 8 ℃/min, preserving heat for 3h, heating to 1750 ℃ at the speed of 6 ℃/min, preserving heat for 4h, then cooling to 1500 ℃ at the speed of 2 ℃/min, preserving heat for 1h, finally cooling to 1300 ℃ at the speed of 5 ℃/min, preserving heat for 0.5h, and furnace-cooling to obtain (La)0.3Tb0.1Dy0.2Ho0.2Er0.2)MgAl11O19A ceramic material.
Comparative example 1
La2O3Powder (average particle diameter of 10nm, purity greater than or equal to 99.9%) and Al2O3Powder (average particle diameter of 10nm, purity greater than or equal to 99.9%) and MgO powder (average particle diameter of 10nm, purity greater than or equal to 99.9%) according to LaMgAl11O19Is dosed in a stoichiometric ratio of (a), wherein La2O3Powder of Al2O3The mol ratio of the powder to the MgO powder is 1:11:2 respectively, the obtained mixture is mixed with absolute ethyl alcohol, and wet ball milling is carried out, wherein the ball milling rotation speed is 300rpm, and the ball milling time is 10 hours, so that white powder which is uniformly mixed is obtained;
putting the white mixed powder into a stainless steel mold, and maintaining the pressure for 2min under the pressure of 2MPa to obtain a cylindrical blank with the diameter of 12 mm;
putting the cylindrical blank into a muffle furnace, heating to 1450 ℃ at the speed of 10 ℃/min, preserving heat for 2h, heating to 1700 ℃ at the speed of 5 ℃/min, preserving heat for 5h, then cooling to 1450 ℃ at the speed of 4 ℃/min, preserving heat for 2h, finally cooling to 1250 ℃ at the speed of 8 ℃/min, preserving heat for 1h, and cooling along with the furnace to obtain LaMgAl11O19Ceramic samples.
Comparative example 2
La2O3Powder (average particle diameter of 10nm, purity greater than or equal to 99.9%) and Al2O3Powder (average particle diameter of 10nm, purity greater than or equal to 99.9%) and MgO powder (average particle diameter of 10nm, purity greater than or equal to 99.9%) according to LaMgAl11O19Is dosed in a stoichiometric ratio of (a), wherein La2O3Powder of Al2O3The mol ratio of the powder to the MgO powder is 1:11:2 respectively, the obtained mixture is mixed with absolute ethyl alcohol, wet ball milling is carried out, the ball milling rotation speed is 280rpm, and the ball milling time is 12 hours, so that white mixed powder is obtained;
putting the white mixed powder into a stainless steel mold, and maintaining the pressure for 4min under the pressure of 1MPa to obtain a cylindrical blank with the diameter of 12 mm;
putting the cylindrical blank into a muffle furnace at the speed of 8 ℃/minHeating to 1400 ℃, keeping the temperature for 3h, heating to 1750 ℃ at the speed of 6 ℃/min, keeping the temperature for 4h, then cooling to 1500 ℃ at the speed of 2 ℃/min, keeping the temperature for 1h, finally cooling to 1300 ℃ at the speed of 5 ℃/min, keeping the temperature for 0.5h, and furnace cooling to obtain LaMgAl11O19Ceramic samples.
Characterization and Performance testing
1) For (La) prepared in example 10.2Tb0.2Dy0.2Ho0.2Er0.2)MgAl11O19The ceramic material was subjected to a thermal stability test using (La) prepared in example 10.2Tb0.2Dy0.2Ho0.2Er0.2)MgAl11O19And (3) putting the sample into a muffle furnace, heating to 1300 ℃ at the speed of 2 ℃/min, annealing for 4h (heat treatment), cooling along with the furnace, mashing the obtained product, and sieving by using a 300-mesh sieve to obtain the heat-treated ceramic powder.
For (La) prepared in example 10.2Tb0.2Dy0.2Ho0.2Er0.2)MgAl11O19XRD test is carried out on the sample before and after the ceramic material is subjected to heat treatment, and the result is shown in figure 1; as can be seen from FIG. 1, the phase structure is a single phase, and no impurity phase exists; moreover, the ceramic material prepared in example 1 has no phase change after annealing treatment at 1300 ℃ for 4 hours, and is consistent with the test result at room temperature (before heat treatment), which shows that the ceramic material prepared in example 1 has high thermal stability;
for (La) prepared in example 10.2Tb0.2Dy0.2Ho0.2Er0.2)MgAl11O19SEM test is carried out on a sample before the ceramic material is subjected to heat treatment, and the result is shown in figure 2; as can be seen from FIG. 2, the ceramic surface was free of microcracks.
2) Adopting the thermal stability test method of the above 1), the LaMgAl prepared by the comparative example 111O19XRD tests are carried out on samples of the ceramic material before and after heat treatment, and the results are shown in figure 3; as can be seen from FIG. 3, LaMgAl was prepared by the same process as in example 111O19The second phase LaAlO is obvious after the annealing treatment3Which indicates the diffraction peak of the present inventionCeramic materials have high thermal stability.
3) For (La) prepared in example 20.3Tb0.1Dy0.2Ho0.2Er0.2)MgAl11O19The ceramic material was subjected to a thermal stability test using (La) prepared in example 20.3Tb0.1Dy0.2Ho0.2Er0.2)MgAl11O19Putting the sample into a muffle furnace, heating to 1200 ℃ at the speed of 5 ℃/min, annealing for 2h (heat treatment), cooling along with the furnace, mashing the obtained product, sieving by using a 200-mesh sieve to obtain heat-treated ceramic powder, and carrying out XRD (X-ray diffraction) test on the sample before and after heat treatment, wherein the result is shown in figure 4; as can be seen from FIG. 4, the ceramic phase structure is a single phase, and no impurity phase exists; also, (La) prepared in example 20.3Tb0.1Dy0.2Ho0.2Er0.2)MgAl11O19After the ceramic is annealed at 1200 ℃ for 2 hours, the phase is not changed, and the test result is consistent with the test result at room temperature (before heat treatment);
for (La) prepared in example 20.3Tb0.1Dy0.2Ho0.2Er0.2)MgAl11O19SEM testing of the ceramic material resulted in figure 5; as can be seen from fig. 5, the sample surface was free of microcracks.
4) Adopting the thermal stability testing method of the 3) to compare the LaMgAl prepared by the comparative example 211O19XRD tests are carried out on samples of the ceramic material before and after heat treatment, and the results are shown in figure 6; as can be seen from FIG. 6, LaMgAl prepared by the same process in comparative example 211O19Under the condition, obvious second phase LaAlO appears after annealing treatment3This indicates that the ceramic material of the present invention has high thermal stability.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. HeightThermally stable ceramic material characterized by a chemical composition of (La)0.4-xTbxDy0.2Ho0.2Er0.2)MgAl11O19Wherein, 0<x≤0.2。
2. The high thermal stability ceramic material of claim 1, wherein x is 0.1 to 0.15.
3. A process for the preparation of a high thermal stability ceramic material according to claim 1 or 2, characterized in that it comprises the following steps:
mixing a lanthanum source, a terbium source, a dysprosium source, a holmium source, an erbium source, a magnesium source and an aluminum source, and performing cold press molding to obtain a blank body; the molar ratio of lanthanum element, terbium element, dysprosium element, holmium element, magnesium element and aluminum element in the lanthanum source, terbium source, dysprosium source, holmium source, erbium element and aluminum source is (0.4-x) x is 0.2:0.2:0.2:1:11, and x is more than 0 and less than or equal to 0.2;
carrying out staged heat preservation on the blank to obtain a high-thermal-stability ceramic material;
the staged heat preservation process comprises the following steps: the first stage is as follows: the calcination temperature is 1400-1450 ℃, and the heat preservation time is 2-3 h; and a second stage: the calcining temperature is 1700-1750 ℃, and the heat preservation time is 4-5 h; and a third stage: the calcination temperature is 1450-1500 ℃, and the heat preservation time is 1-2 h; a fourth stage: the calcination temperature is 1250-1300 ℃, and the heat preservation time is 0.5-1 h.
4. The method of claim 3, wherein the lanthanum source comprises lanthanum oxide; the terbium source comprises terbium oxide; the dysprosium source comprises dysprosium oxide and the holmium source comprises holmium oxide; the erbium source comprises erbium oxide, the magnesium source comprises magnesium oxide, and the aluminum source comprises aluminum oxide.
5. The preparation method according to claim 3 or 4, characterized in that the lanthanum source, the neodymium source, the gadolinium source, the samarium source, the rare earth oxide, the magnesium source and the aluminum source have independent particle sizes of 2-10 nm and independent purities of not less than 99.9%.
6. The preparation method according to claim 3, wherein the pressure of the cold press molding is 1-2 MPa, and the dwell time is 2-4 min.
7. The method according to claim 3, wherein the rate of temperature increase from room temperature to the calcination temperature in the first stage is 8 to 10 ℃/min.
8. The method according to claim 3, wherein a temperature increase rate from the calcination temperature in the first stage to the calcination temperature in the second stage is 5 to 6 ℃/min.
9. The preparation method according to claim 3, wherein the rate of cooling from the calcination temperature of the second stage to the calcination temperature of the third stage is 2 to 4 ℃/min; and the rate of reducing the temperature from the calcining temperature of the third stage to the calcining temperature of the fourth stage is 5-8 ℃/min.
10. Use of the high-stability ceramic material according to claim 1 or 2 or the high-thermal-stability ceramic material prepared by the preparation method according to any one of claims 3 to 9 in the field of thermal protection of aerospace vehicles or in the field of industrial kilns.
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| CN114573346A (en) * | 2022-04-08 | 2022-06-03 | 厦门稀土材料研究所 | Rare earth high-entropy aluminate ceramic selective emitter for thermophotovoltaic and preparation method and application thereof |
| CN116161975A (en) * | 2023-03-22 | 2023-05-26 | 中国地质大学（武汉） | High-entropy thermal barrier coating material with high fracture toughness and hexagonal magnetoplumbite structure and preparation method thereof |
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| CN116161975A (en) * | 2023-03-22 | 2023-05-26 | 中国地质大学（武汉） | High-entropy thermal barrier coating material with high fracture toughness and hexagonal magnetoplumbite structure and preparation method thereof |
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