CN114621004A - High-entropy ceramic material with high energy storage density and preparation method thereof - Google Patents
High-entropy ceramic material with high energy storage density and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-entropy ceramic material with high energy storage density and a preparation method thereof, which adopts a solid-phase synthesis method and uses Bi2O3、Na2CO3、K2CO3、BaCO3、SrCO3、TiO2And Nb2O5Is prepared from Bi0.2Na0.2K0.2Ba0.2Sr0.2)Ti0.8Nb0.2O3Proportioning and taking materials, performing wet ball milling mixing on the powder, performing secondary ball milling on the dried powder after presintering, sieving and pressing, and finally sintering to obtain the perovskite type high-entropy ceramic with high energy storage and high efficiency. The energy storage ceramic material obtained by the invention can restore the energy storage density Wrec＝4.53J/cm3The energy storage efficiency η is 88.1%. The energy storage performance is greatly improved compared with the existing product. In addition, the process flow is simple, the method is suitable for industrial production, and the method meets the current lead-free environment-friendly requirement.
Description
Technical Field
The invention belongs to the field of dielectric energy storage materials, and particularly relates to a high-entropy ceramic material with high energy storage density and a preparation method thereof.
Background
The dielectric ceramic energy storage material in the dielectric capacitor has the characteristics of high power density, low cost, excellent thermal stability and the like, and is widely applied to high-power systems such as commerce, consumption, medical treatment, military and the like. At present, most of materials used for ceramic capacitors are lead-based ceramics, although the energy storage density is high, the systems contain a large amount of lead elements, which has great harm to human health and environment, and the development of lead-free materials to replace lead-containing system materials is a necessary trend. However, the lead-free dielectric ceramic capacitor has a limitation in that the energy storage density is low and cannot be compared with the energy storage performance of a lead-based ceramic capacitor, which makes it difficult to meet the development requirements of miniaturization, multifunction and integration of devices, thereby limiting its application in portable electronic devices. If the energy storage density of the lead-free dielectric ceramic capacitor can be effectively improved, the lead-free dielectric ceramic capacitor can be more widely applied to the field of energy storage.
In recent years, high-entropy materials have received extensive attention and research due to their various excellent mechanical and physical properties, unique structures and potential for development. Over the past few years, there has been considerable progress in the development of high entropy materials, extending from the initial high entropy alloy systems to high entropy ceramic systems such as metal carbides, diborides and oxides. At present, the research on the high-entropy oxide is mainly focused on rock-salt structures, but the research on the high-entropy perovskite is rarely seen. Perovskite oxides (ABO)3) Applications are in many areas such as energy storage, ionic conductors and magneto-resistance. Combining high entropy with perovskite tends to produce unexpected results, but the synthesis of high entropy materials is very muchIt is difficult. By 2018, only a few high entropy ceramics were successfully manufactured in bulk form.
Disclosure of Invention
Aiming at the defects of the technology, the invention aims to provide a high-entropy ceramic material with high energy storage density and a preparation method thereof, wherein a high-entropy structure is constructed by increasing the number of elements on A and B positions in a perovskite structure, so that a novel dielectric material with excellent dielectric property is prepared.
In order to solve the technical problems in the prior art, the technical scheme of the invention is as follows:
a high-entropy ceramic material with high energy storage density has a chemical composition of (Bi)0.2Na0.2K0.2Ba0.2Sr0.2)Ti0.8Nb0.2O3。
As a further improvement scheme, the sintering temperature of the ceramic material is 1150-1200 ℃.
As a further improvement, when the sintering temperature of the ceramic material is 1150 ℃, the charging energy density of the obtained ceramic material under an electric field of 380kV/cm reaches 6.25J/cm3The available energy storage density reaches 3.47J/cm3And the energy storage efficiency reaches 55.5 percent.
As a further improvement, when the sintering temperature of the ceramic material is 1175 ℃, the charging energy density of the obtained ceramic material under an electric field of 340kV/cm reaches 5.14J/cm3The available energy storage density reaches 4.53J/cm3And the energy storage efficiency reaches 88.1 percent.
As a further improvement, when the sintering temperature of the ceramic material is 1200 ℃, the charging energy density of the obtained ceramic material under the electric field of 160kV/cm reaches 1.62J/cm3The available energy storage density reaches 1.31J/cm3And the energy storage efficiency reaches 80.9 percent.
The invention also discloses a preparation method of the perovskite type high-entropy ceramic, which is used for preparing the corresponding energy storage ceramic by a solid-phase reaction method and specifically comprises the following steps:
(1) selecting Bi with the purity of more than 98 percent2O3Powder of Na2CO3Powder of, K2CO3Powder of BaCO3Powder of SrCO3Powder of TiO2Powder of Nb2O5The powder is used as raw material and is represented by the general formula (Bi)0.2Na0.2K0.2Ba0.2Sr0.2)Ti0.8Nb0.2O3Weighing raw materials, adding absolute ethyl alcohol with the same amount as the powder, and uniformly mixing the raw materials through a primary ball milling process to uniformly mix the powder to form slurry;
(2) placing the slurry in a constant-temperature oven at 90 ℃ for baking, removing absolute ethyl alcohol, and grinding in a mortar to obtain powder;
(3) placing the powder in a mould to be pre-pressed into a material block, pre-burning the material block at 750 ℃ under a closed condition, and keeping the temperature for 3-4h to obtain pre-synthesized ceramic powder;
(4) crushing and grinding the pre-synthesized ceramic material block in a mortar to obtain ceramic powder, adding equal amount of absolute ethyl alcohol into the obtained powder, and carrying out secondary ball milling;
(5) drying the obtained slurry at 90 ℃, and performing granulation, sieving and compression molding to obtain a ceramic green body;
(6) carrying out glue discharging treatment on the ceramic blank at the temperature of 600-650 ℃ for 3-4h, sintering the ceramic blank after glue discharging, wherein the sintering temperature is 1150-1200 ℃, the heating rate is 3-4 ℃/min, the heat preservation time is 2-3h, and cooling to room temperature to obtain the perovskite type high-entropy ceramic with high energy storage and high efficiency;
(7) carrying out hot corrosion treatment on the prepared sample, then taking an SEM picture, and observing the compactness degree and the grain size of the ceramic;
(8) processing the prepared sample into a sheet with two smooth surfaces and a thickness of about 0.1mm, plating an electrode with gold, testing the ferroelectric property at the room temperature under the frequency of 10Hz, and calculating the energy storage property;
(9) coating silver paste on two sides of the prepared sample, carrying out silver firing treatment at 565 ℃ for 20min, cooling to room temperature, and then carrying out dielectric property test.
Further, absolute ethyl alcohol and ZrO are adopted in the primary ball milling and the secondary ball milling2Balls as ball-milling mediumThe rotating speed is 225r/min, the running direction is adjusted every half hour, and the ball milling time is 12 h.
Further, the pre-firing temperature is preferably 750 ℃ and the holding time is preferably 4 hours.
Furthermore, polyvinyl alcohol (PVA) with the concentration of 8% is used as a binder to be mixed into the powder during granulation, the mass of the mixed binder is 5% of the mass of the powder, the mass of the mixed distilled water is 2.5% of the mass of the powder, the powder is uniformly mixed in a mortar and then placed in a mold, and the powder is pressed into powder blocks.
Furthermore, sieving with 60 mesh and 140 mesh sieve to obtain powder of middle layer of 60 mesh and 140 mesh sieve.
Further, the pressure at the time of press molding was controlled to 200 MPa.
Further, when the green body is placed in a crucible for glue removal, a gap is reserved between a cover covered on the crucible and the crucible; during sintering, sealed sintering is adopted, and a crucible is inverted on a ceramic green body for sealing.
Furthermore, the heating rate is controlled at 4 ℃/min during sintering, and the heat preservation time is controlled at 2 h.
In principle, high entropy represents an increase in disorder, and also an increase in disorder in which the polarization in the crystal changes from long range ordered ferroelectric domains to polar nanodomains during the transition from ferroelectric to relaxor ferroelectric. According to the invention, bismuth, sodium, potassium, barium and strontium ions are introduced into the A site of the perovskite structure, and titanium and niobium ions are introduced into the B site, so that the perovskite type high-entropy structure is obtained. Finally obtaining the high effective energy storage density of 4.53J/cm3The novel high-entropy perovskite ceramic of (2).
Compared with the prior art, the invention provides a simple and effective method for preparing the perovskite type high-entropy energy storage ceramic, the obtained high-entropy ceramic has a slender hysteresis loop, high energy storage density and energy storage efficiency, has extremely high application value for realizing lead-free of pulse power devices, has great significance for replacing lead-based energy storage ceramic materials, and can be widely applied to pulse power systems such as high-power microwave weapons, laser weapons, electromagnetic transmitters, hybrid electric vehicles and the like.
Drawings
FIG. 1 shows (Bi)0.2Na0.2K0.2Ba0.2Sr0.2)Ti0.8Nb0.2O3The sintering temperature of the ceramic material is 1150 ℃;
FIG. 2 shows (Bi)0.2Na0.2K0.2Ba0.2Sr0.2)Ti0.8Nb0.2O3The sintering temperature of the ceramic material is a dielectric temperature spectrum at 1175 ℃;
FIG. 3 shows (Bi)0.2Na0.2K0.2Ba0.2Sr0.2)Ti0.8Nb0.2O3The sintering temperature of the ceramic material is 1200 ℃ and the dielectric temperature spectrum is obtained;
FIG. 4 shows (Bi)0.2Na0.2K0.2Ba0.2Sr0.2)Ti0.8Nb0.2O3The sintering temperature of the ceramic material is 1150 ℃;
FIG. 5 shows (Bi)0.2Na0.2K0.2Ba0.2Sr0.2)Ti0.8Nb0.2O3The sintering temperature of the ceramic material is a hysteresis loop at 1175 ℃;
FIG. 6 shows (Bi)0.2Na0.2K0.2Ba0.2Sr0.2)Ti0.8Nb0.2O3The sintering temperature of the ceramic material is 1200 ℃.
Detailed Description
The present invention will be described in detail below with reference to the drawings and examples, but the present invention is not limited to the following examples.
In the present invention, (Bi) is prepared0.2Na0.2K0.2Ba0.2Sr0.2)Ti0.8Nb0.2O3A ceramic material.
Example one
The chemical formula of the high-entropy ceramic material is (Bi)0.2Na0.2K0.2Ba0.2Sr0.2)Ti0.8Nb0.2O3The sintering temperature is 1150 ℃.
The preparation method of the ceramic comprises the following steps:
(1) selecting Bi with the purity of more than 98 percent2O3Powder of Na2CO3Powder of, K2CO3Powder of BaCO3Powder of SrCO3Powder of TiO2Powder of Nb2O5The powder is used as raw material and is prepared according to the chemical formula (Bi)0.2Na0.2K0.2Ba0.2Sr0.2)Ti0.8Nb0.2O3Weighing raw materials, adding absolute ethyl alcohol with the same amount as the powder, and uniformly mixing the raw materials and the absolute ethyl alcohol through a primary ball milling process to uniformly mix the powder to form slurry. Wherein, anhydrous ethanol and ZrO are adopted in the primary ball milling2The ball is used as a ball milling medium, the rotating speed is 225r/min, the running direction is adjusted every half hour, and the ball milling time is 12 hours;
(2) placing the slurry in a constant-temperature oven at 90 ℃ for baking, removing absolute ethyl alcohol, and grinding in a mortar to obtain powder;
(3) placing the powder in a mould to be pre-pressed into a material block, pre-sintering the material block at 750 ℃ under a closed condition, and keeping the temperature for 4 hours to obtain pre-synthesized ceramic powder;
(4) grinding the pre-synthesized ceramic material block in a mortar to obtain ceramic powder, adding anhydrous ethanol with the same amount into the obtained ceramic powder, and performing secondary ball milling, wherein the anhydrous ethanol and ZrO are still adopted in the process2The ball is used as a ball milling medium, the rotating speed is 225r/min, the running direction is adjusted every half hour, and the ball milling time is 12 hours;
(5) drying the obtained slurry at 90 ℃, and adding 8 wt% of polyvinyl alcohol (PVA)
And mixing the powder serving as a binder into the powder for granulation, crushing the powder blocks obtained by granulation, sieving the powder blocks by using 60-mesh and 140-mesh sieves, and performing compression molding on the powder blocks in the middle layers of the 60-mesh and 140-mesh sieves under the pressure of 200Mpa to obtain the ceramic green bodies. Wherein, during granulation, the mass of the mixed binder is 5 percent of the mass of the powder, and the mass of the mixed distilled water is 2.5 percent of the mass of the powder;
(6) placing the ceramic blank in a crucible, covering a cover with a gap, carrying out glue discharging treatment at 650 ℃ for 3h, then sintering the ceramic blank after glue discharging, wherein the sintering temperature is 1150 ℃, the heating rate is 4 ℃/min, the heat preservation time is 2h, and cooling to room temperature to obtain high-entropy ceramic with high energy storage density;
(7) the prepared sample is processed into a thin sheet with two smooth surfaces and the thickness of about 0.1mm, an electrode is plated with gold, and then the ferroelectric property of the sample is tested at the room temperature and the frequency of 10Hz, and the energy storage performance is calculated. The charging energy density (total energy density, W) of the ceramic under the 380kV/cm electric field is obtained by calculation to reach 6.25J/cm3Available energy storage density (available energy storage density, W)rec) Reach 3.47J/cm3The energy storage efficiency (eta) reaches 55.5 percent;
(8) coating silver paste on two sides of the prepared sample, carrying out silver firing treatment at 565 ℃ for 20min, cooling to room temperature, and then carrying out dielectric property test. The dielectric constant of the ceramic can be changed along with the change of the temperature environment of the ceramic according to the test result, and the test result shows that the temperature corresponding to the dielectric peak of the ceramic is lower than the room temperature under 1 MHz. No obvious Tc exists in the dielectric temperature spectrum, and the dielectric peak is not obvious sharp.
Example two
The chemical formula of the high-entropy ceramic material is (Bi)0.2Na0.2K0.2Ba0.2Sr0.2)Ti0.8Nb0.2O3The sintering temperature was 1175 ℃.
The preparation method of the ceramic comprises the following steps:
(1) selecting Bi with the purity of more than 98 percent2O3Powder of Na2CO3Powder of, K2CO3Powder of BaCO3Powder of SrCO3Powder of TiO2Powder of Nb2O5The powder is used as raw material and is prepared according to the chemical formula (Bi)0.2Na0.2K0.2Ba0.2Sr0.2)Ti0.8Nb0.2O3Weighing raw materials, adding anhydrous ethanol with the same amount as the powder, and mixing by one-step ball milling process to obtain a mixtureA slurry is formed. Wherein, anhydrous ethanol and ZrO are adopted in the primary ball milling2The ball is used as a ball milling medium, the rotating speed is 225r/min, the running direction is adjusted every half hour, and the ball milling time is 12 hours;
(2) placing the slurry in a constant-temperature oven at 90 ℃ for baking, removing absolute ethyl alcohol, and grinding in a mortar to obtain powder;
(3) placing the powder in a mould to be pre-pressed into a material block, pre-sintering the material block at 750 ℃ under a closed condition, and keeping the temperature for 4 hours to obtain pre-synthesized ceramic powder;
(4) grinding the pre-synthesized ceramic material block in a mortar to obtain ceramic powder, adding anhydrous ethanol with the same amount into the obtained ceramic powder, and performing secondary ball milling, wherein the anhydrous ethanol and ZrO are still adopted in the process2The ball is used as a ball milling medium, the rotating speed is 225r/min, the running direction is adjusted every half hour, and the ball milling time is 12 hours;
(5) drying the obtained slurry at 90 ℃, adding 8 wt% of polyvinyl alcohol (PVA) as a binder to be doped into the powder for granulation, crushing the powder blocks obtained by granulation, sieving the powder blocks by using 60-mesh and 140-mesh sieves, taking the powder blocks in the middle layers of the 60-mesh and 140-mesh sieves, and performing compression molding under the pressure of 200Mpa to obtain the ceramic green bodies. Wherein, during granulation, the mass of the mixed binder is 5 percent of the mass of the powder, and the mass of the mixed distilled water is 2.5 percent of the mass of the powder;
(6) placing the ceramic blank in a crucible, covering a cover with a gap, carrying out glue discharging treatment at 650 ℃ for 3h, then sintering the ceramic blank after glue discharging, wherein the sintering temperature is 1175 ℃, the heating rate is 4 ℃/min, the heat preservation time is 2h, and cooling to room temperature to obtain the perovskite type high-entropy ceramic with high energy storage and high efficiency;
(7) the prepared sample is processed into a thin sheet with two smooth surfaces and the thickness of about 0.1mm, an electrode is plated with gold, and then the ferroelectric property of the sample is tested at the room temperature and the frequency of 10Hz, and the energy storage performance is calculated. The charging energy density (total energy density, W) of the ceramic under the 340kV/cm electric field is calculated to reach 5.14J/cm3Available energy storage density (available energy storage density, W)rec) Reaching 4.53J/cm3The energy storage efficiency (eta) reaches 88.1 percent;
(8) coating silver paste on two sides of the prepared sample, carrying out silver firing treatment at 565 ℃ for 20min, cooling to room temperature, and then carrying out dielectric property test. The test result shows that the dielectric constant of the ceramic changes along with the change of the temperature environment where the ceramic is located, and the test result shows that the temperature corresponding to the dielectric peak of the ceramic is lower than the room temperature under 1 MHz. No obvious Tc exists in the dielectric temperature spectrum, and the dielectric peak is not obvious sharp.
EXAMPLE III
The chemical formula of the high-entropy ceramic material is (Bi)0.2Na0.2K0.2Ba0.2Sr0.2)Ti0.8Nb0.2O3The sintering temperature was 1200 ℃.
The preparation method of the ceramic comprises the following steps:
(1) selecting Bi with the purity of more than 98 percent2O3Powder of Na2CO3Powder of, K2CO3Powder of BaCO3Powder of SrCO3Powder of TiO2Powder of Nb2O5The powder is used as raw material and is prepared according to the chemical formula (Bi)0.2Na0.2K0.2Ba0.2Sr0.2)Ti0.8Nb0.2O3Weighing raw materials, adding absolute ethyl alcohol with the same amount as the powder, and uniformly mixing the raw materials and the absolute ethyl alcohol through a primary ball milling process to uniformly mix the powder to form slurry. Wherein, anhydrous ethanol and ZrO are adopted in the primary ball milling2The ball is used as a ball milling medium, the rotating speed is 225r/min, the running direction is adjusted every half hour, and the ball milling time is 12 hours;
(2) placing the slurry in a constant-temperature oven at 90 ℃ for baking, removing absolute ethyl alcohol, and grinding in a mortar to obtain powder;
(3) placing the powder in a mould to be pre-pressed into a material block, pre-sintering the material block at 750 ℃ under a closed condition, and keeping the temperature for 4 hours to obtain pre-synthesized ceramic powder;
(4) grinding the pre-synthesized ceramic material block in a mortar to obtain ceramic powder, adding equal amount of absolute ethyl alcohol into the obtained powder, performing secondary ball milling,the anhydrous ethanol and ZrO are still adopted in the process2The ball is used as a ball milling medium, the rotating speed is 225r/min, the running direction is adjusted every half hour, and the ball milling time is 12 hours;
(5) drying the obtained slurry at 90 ℃, adding 8 wt% of polyvinyl alcohol (PVA) as a binder to be doped into the powder for granulation, crushing the powder blocks obtained by granulation, sieving the powder blocks by using 60-mesh and 140-mesh sieves, taking the powder blocks in the middle layers of the 60-mesh and 140-mesh sieves, and performing compression molding under the pressure of 200Mpa to obtain the ceramic green bodies. Wherein, during granulation, the mass of the mixed binder is 5 percent of the mass of the powder, and the mass of the mixed distilled water is 2.5 percent of the mass of the powder;
(6) placing the ceramic blank in a crucible, covering a cover with a gap, carrying out glue discharging treatment at 650 ℃ for 3h, then sintering the ceramic blank after glue discharging, wherein the sintering temperature is 1200 ℃, the heating rate is 4 ℃/min, the heat preservation time is 2h, and cooling to room temperature to obtain high-entropy ceramic with high energy storage density;
(7) the prepared sample is processed into a thin sheet with two smooth surfaces and the thickness of about 0.1mm, an electrode is plated with gold, and then the ferroelectric property of the sample is tested at the room temperature and the frequency of 10Hz, and the energy storage performance is calculated. The charging energy density (total energy density, W) of the ceramic under the electric field of 160kV/cm reaches 1.62J/cm3Available energy storage density (available energy storage density, W)rec) Reaching 1.31J/cm3The energy storage efficiency (eta) reaches 80.9 percent;
(8) coating silver paste on two sides of the prepared sample, carrying out silver firing treatment at 565 ℃ for 20min, cooling to room temperature, and then carrying out dielectric property test. The test result shows that the dielectric constant of the ceramic changes along with the change of the temperature environment where the ceramic is located, and the test result shows that the temperature corresponding to the dielectric peak of the ceramic is lower than the room temperature under 1 MHz. No obvious Tc exists in the dielectric temperature spectrum, and the dielectric peak is not obvious sharp.
Referring to FIG. 1, FIG. 2, and FIG. 3 are respectively the dielectric constant versus temperature curves at 1MHz for the samples prepared in the above examples.
Referring to fig. 4, fig. 5, and fig. 6 respectively show the energy storage performance of the samples prepared in the above examples in an electric field.
The embodiments described above are intended to facilitate the 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 (10)
1. A high-entropy ceramic material with high energy storage density is characterized in that the chemical composition of the ceramic material is (Bi)0.2Na0.2K0.2Ba0.2Sr0.2)Ti0.8Nb0.2O3。
2. The high-entropy ceramic material with high energy storage density of claim 1, wherein the sintering temperature of the ceramic material is 1150-1200 ℃.
3. The high-entropy ceramic material with high energy storage density of claim 2, wherein the ceramic material obtained has a charging energy density of 6.25J/cm under an electric field of 380kV/cm at a sintering temperature of 1150 ℃ under the condition that the charging energy density of the ceramic material is up to 6.25J/cm3The available energy storage density reaches 3.47J/cm3And the energy storage efficiency reaches 55.5 percent.
4. The high-entropy ceramic material with high energy storage density of claim 2, wherein the ceramic material has a sintering temperature of 1175 ℃ and a charging energy density of 5.14J/cm under an electric field of 340kV/cm3The available energy storage density reaches 4.53J/cm3And the energy storage efficiency reaches 88.1 percent.
5. A high-entropy ceramic material with high energy storage density according to claim 2, wherein the sintering temperature of the ceramic material is 1200 ℃ to obtain a ceramic materialThe charging energy density under the 160kV/cm electric field reaches 1.62J/cm3The available energy storage density reaches 1.31J/cm3And the energy storage efficiency reaches 80.9 percent.
6. A preparation method of a high-entropy ceramic material with high energy storage density is characterized in that a solid-phase reaction method is used for preparing corresponding energy storage ceramic, and the method specifically comprises the following steps:
selecting Bi with the purity of more than 98 percent2O3Powder of Na2CO3Powder of, K2CO3Powder of BaCO3Powder of SrCO3Powder of TiO2Powder of Nb2O5The powder is used as a raw material and is prepared according to the general formula (Bi)0.2Na0.2K0.2Ba0.2Sr0.2)Ti0.8Nb0.2O3Weighing raw materials, adding absolute ethyl alcohol with the same amount as the powder, and uniformly mixing the raw materials through a primary ball milling process to uniformly mix the powder to form slurry;
placing the slurry in a constant-temperature oven at 90 ℃ for baking, removing absolute ethyl alcohol, and grinding in a mortar to obtain powder;
placing the powder in a mould to be pre-pressed into a material block, pre-sintering the material block at 750 ℃ under a closed condition, and keeping the temperature for 3-4h to obtain pre-synthesized ceramic powder;
crushing and grinding the pre-synthesized ceramic material block in a mortar to obtain ceramic powder, adding equal amount of absolute ethyl alcohol into the obtained powder, and carrying out secondary ball milling;
drying the obtained slurry at 90 ℃, and performing granulation, sieving and compression molding to obtain a ceramic green body;
carrying out glue discharging treatment on the ceramic blank at the temperature of 600-650 ℃ for 3-4h, sintering the ceramic blank after glue discharging, wherein the sintering temperature is 1150-1200 ℃, the heating rate is 3-4 ℃/min, the heat preservation time is 2-4h, and cooling to the room temperature to obtain the high-entropy perovskite high-energy-density ceramic.
7. The method for preparing high-entropy ceramic material with high energy storage density according to claim 6, wherein the first ball milling and the second ball milling are performedAnhydrous ethanol and ZrO are adopted during secondary ball milling2The ball is used as a ball milling medium, the rotating speed is 225r/min, the running direction is adjusted every half hour, and the ball milling time is 12 h.
8. The method for preparing a high-entropy ceramic material with high energy storage density according to claim 5, wherein polyvinyl alcohol with a concentration of 8% is used as a binder to be mixed into powder during granulation, the mass of the mixed binder is 5% of the mass of the powder, the mass of the mixed distilled water is 2.5% of the mass of the powder, and the powder is uniformly mixed in a mortar, placed in a mold and pressed into a powder block.
9. The method for preparing a high-entropy ceramic material with high energy storage density as claimed in claim 5, wherein when the green body is placed in a crucible for binder removal, a gap is left between a cover covering the crucible and the crucible; during sintering, sealed sintering is adopted, and a crucible is inverted and sealed on the ceramic green body.
10. The preparation method of the high-entropy ceramic material with high energy storage density according to claim 5, wherein the heating rate during sintering is preferably 4 ℃/min, and the heat preservation time is 2 h;
sieving with 60 mesh and 140 mesh sieve, and collecting powder of middle layer of 60 mesh and 140 mesh sieve;
the pressure during the compression molding was controlled at 200 MPa.
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