CN111484325A - Barium strontium titanate-based ceramic material and preparation method and application thereof - Google Patents

Barium strontium titanate-based ceramic material and preparation method and application thereof Download PDF

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CN111484325A
CN111484325A CN202010326200.1A CN202010326200A CN111484325A CN 111484325 A CN111484325 A CN 111484325A CN 202010326200 A CN202010326200 A CN 202010326200A CN 111484325 A CN111484325 A CN 111484325A
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ceramic material
strontium titanate
barium strontium
based ceramic
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庞利霞
周陈
周迪
刘卫国
张磊
王欣
纪红芬
邓立儿
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Xian Technological University
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Abstract

The invention provides a barium strontium titanate-based ceramic material and a preparation method and application thereof, belonging to the technical field of energy storage ceramic materials. The chemical composition of the barium strontium titanate-based ceramic material provided by the invention is (1-x) Ba 0.8Sr0.2TiO3‑xBi(Mg2/3Nb1/3)O3Wherein x is more than or equal to 0.08 and less than or equal to 0.16. The barium strontium titanate-based ceramic material provided by the invention has high energy storage density and energy storage efficiency. The results of the examples show that the barium strontium titanate-based ceramic material provided by the invention has high dielectric relaxation property and breakdown-resistant electric field, and can obtain a slender electric hysteresis loop; under the external electric field of 250kV/cm, the effective energy storage density of the barium strontium titanate-based ceramic material is 2.028J/cm 3And meanwhile, the energy storage efficiency reaches 96.8 percent.

Description

Barium strontium titanate-based ceramic material and preparation method and application thereof
Technical Field
The invention relates to the technical field of energy storage ceramic materials, in particular to a barium strontium titanate-based ceramic material and a preparation method and application thereof.
Background
With the rapid development of world economy and human society, the demand of people on energy is increasing day by day, novel clean energy such as solar energy, wind energy and the like with intermittent type nature, randomness, volatility and other problems is gradually towards the practicality, and the research of using advanced energy storage equipment and technology to reasonably store and utilize the novel renewable energy is also deepened gradually. The dielectric capacitor is very suitable for the field with large power fluctuation or high power density requirement due to the ultrahigh power density and the ultra-fast charge and discharge capacity. In addition, the dielectric capacitor has an extremely rapid charge and discharge process, a long cycle life, and high safety, and thus is widely used in the fields of commerce, medical treatment, military use, and the like. Currently, commercially used dielectric capacitors are primarily ceramic dielectrics with energy densities less than 2J/cm 3As power electronic devices and systems are being developed toward miniaturization, weight reduction, and integration, it is important to develop a dielectric capacitor having a high energy storage density.
The performance of the energy storage ceramic mainly depends on two factors of the dielectric constant and the insulativity of the energy storage ceramic, and the energy storage characteristic of the ceramic dielectric has a direct proportional relation with the product of the dielectric constant and the square of the working field intensity. BaTiO 2 3The ceramic is used as an energy storage ceramic, and the energy storage density of the ceramic is restricted due to the lower breakdown field strength, the larger remanent polarization and the lower energy storage efficiency of the ceramic. At the same time, BaTiO 3The ceramics also have electrostrictive phenomenon, and internal cracks are easy to generate when the ceramics work in an alternating electric field.
The strontium titanate-based material and the barium titanate-based material belong to ABO 3Perovskite compounds, and both of them have excellent photoelectric characteristics. Barium titanate is a standard ferroelectric and the phase change can occur as a ferroelectric to paraelectric transition. Strontium titanate at normal temperature is paraelectric and has high dielectric constant at low temperature. From barium titanate Barium strontium titanate ((Ba, Sr) TiO) formed by solid solution with strontium titanate in any proportion 3) The material shows good electrical and optical properties. (Ba, Sr) TiO 3The dielectric constant is high, the loss is low, the stability is good, different Ba/Sr ratios can be prepared, and the preparation method is beneficial to being used under various harsh conditions and environments. But (Ba, Sr) TiO 3The energy storage performance of (a) still remains to be improved.
Disclosure of Invention
The invention aims to provide a barium strontium titanate-based 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 barium strontium titanate-based ceramic material, the chemical composition of which is (1-x) Ba 0.8Sr0.2TiO3-xBi(Mg2/3Nb1/3)O3Wherein x is more than or equal to 0.08 and less than or equal to 0.16.
Preferably, the barium strontium titanate-based ceramic material has a perovskite structure.
The invention provides a preparation method of the barium strontium titanate-based ceramic material in the technical scheme, which comprises the following steps:
Mixing BaCO 3、Bi2O3、Nb2O5、MgO、SrCO3And TiO 2And (3) preparing the materials according to the chemical composition of the barium strontium titanate-based ceramic material, and then sequentially carrying out primary ball milling, pre-sintering, secondary ball milling, granulation and tabletting, glue discharging and sintering to obtain the barium strontium titanate-based ceramic material.
Preferably, the pre-sintering temperature is 900-920 ℃, and the heat preservation time is 4-6 h.
Preferably, the granulation and tabletting specifically comprises mixing the material obtained after the second ball milling with a binder, granulating, and then pressing the obtained granules to obtain a green body.
Preferably, the particle size of the particles obtained after granulation is 120-250 μm.
Preferably, the pressure of the pressing is 20MPa, and the pressure maintaining time is 50-90 s; the thickness of unburned bricks is 1.0-1.4 mm.
Preferably, the temperature of the rubber discharge is 500-600 ℃, and the heat preservation time is 4-5 h.
Preferably, the sintering temperature is 1280-1300 ℃, and the heat preservation time is 4-6 h.
The invention provides an application of the barium strontium titanate-based ceramic material prepared by the technical scheme or the barium strontium titanate-based ceramic material prepared by the preparation method in the technical scheme in a dielectric capacitor.
The invention provides a barium strontium titanate-based ceramic material, the chemical composition of which is (1-x) Ba 0.8Sr0.2TiO3-xBi(Mg2/3Nb1/3)O3Wherein x is more than or equal to 0.08 and less than or equal to 0.16. In the present invention, Ba 0.8Sr0.2TiO3Phase as the main phase, Bi (Mg) 2/3Nb1/3)O3The phase is a doped secondary phase, x is limited in the range, and the doped secondary phase in the barium strontium titanate-based ceramic material can completely enter the crystal structure of the main phase and be completely dissolved, so that the barium strontium titanate-based ceramic material has a perovskite structure and has no impurity phase; in addition, the doped auxiliary phase is introduced on the basis of the main phase, and the density of the main phase is favorably improved and the content of air holes is reduced by regulating the proportion of each component within the range, so that the effect of improving the breakdown field intensity is achieved, and the barium strontium titanate-based ceramic material is ensured to have excellent energy storage characteristics. The results of the examples show that the barium strontium titanate-based ceramic material provided by the invention has high dielectric relaxation property and breakdown-resistant electric field, and can obtain a slender electric hysteresis loop; under the external electric field of 250kV/cm, the effective energy storage density of the barium strontium titanate-based ceramic material is 2.028J/cm 3And meanwhile, the energy storage efficiency reaches 96.8 percent.
Drawings
FIG. 1 is an XRD pattern of the barium strontium titanate-based ceramic material prepared in examples 1 to 5;
Fig. 2 is an SEM image of the barium strontium titanate-based ceramic material prepared in example 1;
FIG. 3 shows the results of 0.92Ba in example 1 0.8Sr0.2TiO3-0.08Bi(Mg2/3Nb1/3)O3The prepared ceramic element has a hysteresis loop at room temperature;
FIG. 4 shows the results of 0.9Ba in example 2 0.8Sr0.2TiO3-0.1Bi(Mg2/3Nb1/3)O3The prepared ceramic element has a hysteresis loop at room temperature;
FIG. 5 shows the results of 0.88Ba in example 3 0.8Sr0.2TiO3-0.12Bi(Mg2/3Nb1/3)O3The prepared ceramic element has a hysteresis loop at room temperature;
FIG. 6 shows the results of 0.86Ba in example 4 0.8Sr0.2TiO3-0.14Bi(Mg2/3Nb1/3)O3The prepared ceramic element has a hysteresis loop at room temperature;
FIG. 7 shows the results of 0.84Ba in example 5 0.8Sr0.2TiO3-0.16Bi(Mg2/3Nb1/3)O3The prepared ceramic element has an electric hysteresis loop under the condition of room temperature.
Detailed Description
The invention provides a barium strontium titanate-based ceramic material, the chemical composition of which is (1-x) Ba 0.8Sr0.2TiO3-xBi(Mg2/3Nb1/3)O3Wherein x is more than or equal to 0.08 and less than or equal to 0.16; in the present invention, x may be specifically 0.08, 0.10, 0.12, 0.14 or 0.16, and is preferably 0.10.
In the present invention, the (1-x) Ba 0.8Sr0.2TiO3-xBi(Mg2/3Nb1/3)O3Can be abbreviated as (1-x) BST-xBMN, wherein BST represents Ba 0.8Sr0.2TiO3The main phase is selected; BMN stands for Bi (Mg) 2/3Nb1/3)O3And is a doped secondary phase. The invention limits x in the above range, the secondary phase BMN doped in the barium strontium titanate-based ceramic material can completely enter the crystal structure of the main phase BST and be completely dissolved, so the barium strontium titanate-based ceramic material shows a perovskite structure and has no impurity phase; in addition, the invention introduces the doping auxiliary phase BMN on the basis of the main phase BST, and regulates the component proportion Within the range, the compactness of BST is improved, the content of air holes is reduced, the effect of improving the breakdown field intensity is achieved, and the high energy storage density is finally obtained.
The invention provides a preparation method of the barium strontium titanate-based ceramic material in the technical scheme, which comprises the following steps:
Mixing BaCO 3、Bi2O3、Nb2O5、MgO、SrCO3And TiO 2And (3) preparing the materials according to the chemical composition of the barium strontium titanate-based ceramic material, and then sequentially carrying out primary ball milling, pre-sintering, secondary ball milling, granulation and tabletting, glue discharging and sintering to obtain the barium strontium titanate-based ceramic material.
The invention uses BaCO 3、Bi2O3、Nb2O5、MgO、SrCO3And TiO 2And (3) mixing the materials according to the chemical composition of the barium strontium titanate-based ceramic material to obtain a mixed raw material. According to the invention, the mass of each raw material is preferably weighed by using an electronic balance according to the chemical composition of the barium strontium titanate-based ceramic material, the electronic balance is preferably calibrated and cleared before use, and the reading error is five thousandth so as to ensure precise weighing.
After the ingredients are mixed, the mixed raw materials are subjected to first ball milling to obtain a ball milling mixture. In the invention, the first ball milling is preferably wet milling, the medium used for the wet milling is preferably ethanol, and the milling balls used for the wet milling are preferably zirconium balls; the mass ratio of the zirconium balls to the ethanol to the mixed raw materials is preferably 1.8-2.2: 0.8-2.2: 1, and more preferably 2:1: 1; the rotation speed of the ball mill is preferably 380-420 rpm, and more preferably 400 rpm; the ball milling time is preferably 3.5-4.5 h, and more preferably 4 h. After the first ball milling is finished, the zirconium balls are preferably separated from the obtained slurry, and the slurry is dried to obtain a ball milling mixture. In the invention, the drying temperature is preferably 80-85 ℃; the drying time is not specially limited, and the full drying is ensured. In the invention, in the first ball milling process, the temperature of the mixed raw materials is locally increased in the collision process, thereby accelerating the movement of defects and atoms in the crystal, realizing the refinement of crystal grains and ensuring the smooth proceeding of the subsequent presintering.
After the first ball milling is finished, the ball milling mixture is presintered to obtain a presintering material. In the invention, the pre-sintering temperature is preferably 900-920 ℃, more preferably 910-920 ℃, and the heat preservation time is preferably 4-6 hours, more preferably 4-5 hours; the heating rate from the room temperature to the temperature required by the pre-sintering is preferably 2.5-3.5 ℃/min, and more preferably 3 ℃/min; in the present invention, the pre-firing is preferably performed in an air atmosphere; after the pre-sintering, the present invention is preferably naturally cooled to room temperature. In the embodiment of the invention, the ball-milling mixture is placed in a crucible, compacted and placed in a muffle furnace for pre-sintering; and after the pre-sintering is finished, naturally cooling to room temperature, and taking out the crucible to obtain the pre-sintered material. In the invention, in the pre-sintering process, the oxide raw materials are pre-reacted, so that a required crystal phase is formed through subsequent sintering, and impurities are removed, thereby being beneficial to improving the purity of the product; the invention preferably presintering under the above conditions, can reduce the difficulty of the subsequent sintering process, and is beneficial to saving the cost.
After the pre-sintering is finished, carrying out secondary ball milling on the obtained pre-sintering material; in the present invention, the operation conditions of the second ball milling are preferably consistent with the selectable range of the operation conditions of the first ball milling, and are not described herein again. The invention preferably realizes the refinement of the pre-sintered material through the second ball milling, which is beneficial to more full reaction of each component in the subsequent sintering process.
After the second ball milling is finished, granulating and tabletting the obtained ball-milled material; according to the invention, the ball-milling material is preferably sieved and then granulated and tabletted, the aperture of the sieve for sieving is preferably 60-120 meshes, and undersize materials are taken for granulation and tabletting. In the present invention, the granulation and tableting is preferably carried out by mixing the sieved undersize with a binder, granulating, and then compressing the obtained granules to obtain a green compact.
The invention has no special limitation on the type of the binder, and the binder is well known to those skilled in the art; in the present invention, the binder is preferably a polyvinyl alcohol solution, polyvinyl acetate, or paraffin, more preferably a polyvinyl alcohol solution; in the invention, the mass concentration of the polyvinyl alcohol solution is preferably 4.5-5.5 wt%, and more preferably 5 wt%; the solvent of the polyvinyl alcohol solution is preferably water, and more preferably deionized water; the dosage of the polyvinyl alcohol solution is preferably 5-8% of the mass of the undersize, and more preferably 5%. In the invention, the granularity of the granules obtained after granulation is preferably 120-250 μm; the specific method for granulating is not particularly limited, and the granules with the granularity meeting the requirement can be obtained, specifically, the granules are sieved after granulation, and granules between 60 meshes and 120 meshes are selected for subsequent pressing.
After the granulation is completed, in order to improve the plasticity of the obtained granules, the granules are preferably sealed and stored for 12 hours and then are compressed. In the invention, the pressure intensity of the pressing is preferably 20MPa, the pressure maintaining time is preferably 50-90 s, and more preferably 50-70 s; the thickness of the green body is preferably 1.0-1.4 mm. The invention preferably carries out pressing under the conditions, can compact the blank, is beneficial to discharging air holes in the blank during subsequent sintering, reduces the porosity and further improves the product quality. In the embodiment of the invention, the particles after being sealed and stored for 12 hours are filled into a die and then pressed by a hydraulic press; the specification of the mold is preferably
Figure BDA0002463305270000051
After pressing is finished, the obtained green body is subjected to rubber discharge to obtain a rubber discharge blank. In the invention, the temperature of the rubber discharge is preferably 500-600 ℃, more preferably 500-550 ℃, and the heat preservation time is preferably 4-5 h, more preferably 5 h; the heating rate from room temperature to the temperature required by glue discharging is preferably 1.5-2.5 ℃/min, and more preferably 2 ℃/min; in the present invention, the binder removal is preferably performed in an air atmosphere; after the binder removal, the present invention preferably heats directly for subsequent sintering. In the embodiment of the invention, the green body is placed on a sintering plate (a plurality of green body samples can be processed at one time), and is placed into a box type sintering furnace for glue discharging. According to the invention, the binder in the green body can be rapidly discharged by preferably discharging the binder under the above conditions, so that the subsequent sintering can be smoothly carried out.
After the binder removal is finished, the obtained binder removal blank is sintered to obtain the barium strontium titanate-based ceramic material. In the invention, the sintering temperature is preferably 1280-1300 ℃, and the heat preservation time is preferably 4-6 h, more preferably 4 h; the heating rate from room temperature to the temperature required by sintering is preferably 2-4 ℃/min, and more preferably 3 ℃/min; in the present invention, the sintering is preferably performed in an air atmosphere; after sintering, the present invention is preferably naturally cooled to room temperature. In the embodiment of the invention, the binder removal blank is placed in a sintering furnace for sintering; and naturally cooling to room temperature after sintering, and taking out to obtain the barium strontium titanate-based ceramic material. In the invention, the components fully undergo solid-state reaction in the sintering process, and finally the chemical composition of (1-x) Ba is formed 0.8Sr0.2TiO3-xBi(Mg2/3Nb1/3)O3(wherein x is more than or equal to 0.08 and less than or equal to 0.16) by using a barium strontium titanate-based ceramic material; the invention preferably carries out sintering under the conditions, can ensure that the sintering cost is reduced on the basis of full solid-state reaction of all components, and is beneficial to industrial production.
The invention adopts a solid phase method for sintering, and successfully prepares the barium strontium titanate-based ceramic material with low loss, less defects, high density, good crystallinity and uniform grain size; furthermore, the barium strontium titanate-based energy storage ceramic material can be obtained under conventional pressureless sintering by controlling and adjusting components and selecting proper process parameters, and the method is simple to operate and low in cost.
The invention provides an application of the barium strontium titanate-based ceramic material prepared by the technical scheme or the barium strontium titanate-based ceramic material prepared by the preparation method in the technical scheme in a dielectric capacitor.
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
The composition of the barium strontium titanate-based ceramic material is 0.92Ba 0.8Sr0.2TiO3-0.08Bi(Mg2/3Nb1/3)O3The preparation method comprises the following steps:
(1) Preparing materials: according to the proportion of the formula, calculating BaCO 3、Bi2O3、Nb2O5、MgO、SrCO3And TiO 2Weighing the required mass of each raw material by using a precision electronic balance, and carrying out calibration and zero clearing before using the electronic balance, wherein the reading error is five per thousand;
(2) Primary ball milling: putting zirconium balls, ethanol and a medicine (namely a mixture of the raw materials) into a grinding tank according to the mass ratio of 2:1:1, setting the rotating speed of a ball mill to be 400rpm, carrying out ball milling for 4 hours, separating the zirconium balls after the ball milling is finished, and drying the obtained slurry at 80 ℃ to obtain a ball-milling mixture;
(3) Pre-burning: adding the ball-milling mixture into a crucible, compacting, placing in a muffle furnace, heating from room temperature to 920 ℃ at the speed of 3 ℃/min, and then preserving heat for 4h for pre-sintering; after the pre-sintering is finished, naturally cooling to room temperature, and taking out the crucible to obtain a pre-sintered material;
(4) Secondary ball milling: loading zirconium balls, ethanol and a medicament (namely a pre-sintering material) into a grinding tank according to the mass ratio of 2:1:1, setting the rotating speed of a ball mill to 400rpm, carrying out ball milling for 4 hours, separating the zirconium balls after the ball milling is finished, drying the obtained slurry at 80 ℃, sieving by a 120-mesh sieve, and taking powder under the sieve for subsequent treatment;
(5) Granulating and tabletting: adding a polyvinyl alcohol aqueous solution (the concentration is 5 wt%, the dosage of the polyvinyl alcohol aqueous solution is 5% of the mass of the undersize powder) into the undersize powder for granulation, sieving by a double-layer sieve of 60 meshes and 120 meshes, selecting particles between 60 meshes and 120 meshes, sealing and storing the particles for 12 hours, and then using a die (the specification is that the particles are in accordance with the specification)
Figure BDA0002463305270000071
) And pressing by a hydraulic press to obtain a green body with the thickness of 1.4mm, wherein, The pressure is 20MPa, and the pressure maintaining time is 50 s;
(6) Rubber discharging: placing the green body on a sintering plate, placing the green body in a box type sintering furnace, heating the green body from room temperature to 550 ℃ at the speed of 2 ℃/min, and then preserving heat for 5 hours to carry out rubber discharge to obtain a rubber discharge blank;
(7) And (3) sintering: and putting the binder removal blank into a sintering furnace, heating the blank from room temperature to 1300 ℃ at the speed of 3 ℃/min, then preserving the heat for 4 hours for sintering, and naturally cooling the blank to the room temperature after sintering is finished to obtain the barium strontium titanate-based ceramic material.
Example 2
A barium strontium titanate-based ceramic material was prepared according to the method of example 1, except that the chemical composition of the barium strontium titanate-based ceramic material was 0.9Ba 0.8Sr0.2TiO3-0.1Bi(Mg2/3Nb1/3)O3
Example 3
A barium strontium titanate-based ceramic material was prepared according to the method of example 1, except that the chemical composition of the barium strontium titanate-based ceramic material was 0.88Ba 0.8Sr0.2TiO3-0.12Bi(Mg2/3Nb1/3)O3
Example 4
A barium strontium titanate-based ceramic material was prepared according to the method of example 1, except that the chemical composition of the barium strontium titanate-based ceramic material was 0.86Ba 0.8Sr0.2TiO3-0.14Bi(Mg2/3Nb1/3)O3
Example 5
A barium strontium titanate-based ceramic material was prepared according to the method of example 1, except that the chemical composition of the barium strontium titanate-based ceramic material was 0.84Ba 0.8Sr0.2TiO3-0.16Bi(Mg2/3Nb1/3)O3
The barium strontium titanate-based ceramic materials prepared in examples 1 to 5 were subjected to crystal phase detection by X-ray diffraction analysis (XRD). As shown in figure 1, the XRD diffraction pattern of the (1-x) BST-xBMN ceramic material is that the doping secondary phase BMN completely enters the crystal structure of the main phase BST and is completely dissolved, so that the perovskite structure is shown and no impurity phase exists. Furthermore, as can be seen from FIG. 1, a complete solid solution can be formed when BMN is incorporated in a molar amount of 0.16 or less (x 0.16 or less); as the amount of BMN incorporation increases, the diffraction peak shifts first to a low angle, reaches a minimum at x of 0.10, and then shifts again to a high angle.
Fig. 2 is an SEM image of the barium strontium titanate-based ceramic material prepared in example 1, and it can be seen from fig. 2 that the barium strontium titanate-based ceramic material has uniformly distributed grains, a compact and dense structure, a nearly zero porosity, no common defects, and no excessively grown large grains.
The barium strontium titanate-based ceramic material prepared in the embodiment 1-5 is prepared into a ceramic element, and then a ferroelectric property test is performed, specifically as follows:
Polishing, cleaning and drying the barium strontium titanate-based ceramic material (in a sheet shape) prepared in the embodiment 1-5, respectively coating silver on two surfaces of the obtained ceramic material twice, then placing the ceramic material into a sintering furnace, heating the ceramic material from room temperature to 600 ℃ at the speed of 1 ℃/min, preserving the heat for 60min to enable the silver paste to be uniformly covered on the surface of the ceramic material, then naturally cooling the ceramic material to the room temperature, taking out a sample, and polishing away redundant silver paste on the periphery of the sample by using sand paper to obtain a ceramic element;
The ferroelectric properties of the ceramic element were tested at room temperature (25 ℃) under different electric field conditions, and the obtained hysteresis loops are shown in fig. 3 to 7, and the specific data are listed in table 1.
TABLE 1 results of ferroelectric property test of ceramic device prepared based on barium strontium titanate-based ceramic material in examples 1 to 5
Figure BDA0002463305270000081
Figure BDA0002463305270000091
As shown in FIGS. 3 to 7 and Table 1, the hysteresis loop gradually changed from "fat" to "thin" with increasing x content, the performance was best at x equal to 0.10, and 2.028J/cm could be obtained at a breakdown field of 250kV/cm 3Effective energy storage density The energy storage efficiency was 96.8%.
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. The barium strontium titanate-based ceramic material is characterized by having a chemical composition of (1-x) Ba 0.8Sr0.2TiO3-xBi(Mg2/ 3Nb1/3)O3Wherein x is more than or equal to 0.08 and less than or equal to 0.16.
2. The barium strontium titanate-based ceramic material according to claim 1, wherein the barium strontium titanate-based ceramic material has a perovskite structure.
3. A method for preparing a barium strontium titanate-based ceramic material according to claim 1 or 2, comprising the steps of:
Mixing BaCO 3、Bi2O3、Nb2O5、MgO、SrCO3And TiO 2And (3) preparing the materials according to the chemical composition of the barium strontium titanate-based ceramic material, and then sequentially carrying out primary ball milling, presintering, secondary ball milling, granulation, tabletting, binder removal and sintering to obtain the barium strontium titanate-based ceramic material.
4. The preparation method according to claim 3, wherein the pre-sintering temperature is 900-920 ℃, and the heat preservation time is 4-6 h.
5. The preparation method according to claim 3, wherein the granulation and tabletting is to mix the materials obtained after the second ball milling with a binder and granulate the mixture, and then to compress the obtained granules to obtain a green body.
6. The method according to claim 5, wherein the particle size of the granulated particles is 120 to 250 μm.
7. The production method according to claim 5, wherein the pressure of the pressing is 20MPa and the dwell time is 50 to 90 s; the thickness of unburned bricks is 1.0-1.4 mm.
8. The preparation method according to claim 3, wherein the temperature of the binder removal is 500-600 ℃, and the holding time is 4-5 h.
9. The preparation method according to claim 3, wherein the sintering temperature is 1280-1300 ℃ and the holding time is 4-6 h.
10. The barium strontium titanate-based ceramic material according to claim 1 or 2 or the barium strontium titanate-based ceramic material prepared by the preparation method according to any one of claims 3 to 9 is applied to a dielectric capacitor.
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CN111848199A (en) * 2020-08-11 2020-10-30 长兴鑫原耐火材料科技有限公司 High-thermal-shock long-service-life sagger and preparation method thereof
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CN112919903A (en) * 2021-03-09 2021-06-08 杭州电子科技大学 Strontium bismuth titanate-based lead-free ceramic material for high-efficiency capacitor and preparation method thereof
CN114349497A (en) * 2021-12-28 2022-04-15 摩比天线技术(深圳)有限公司 Wide-temperature-range stable energy storage ceramic material and preparation method thereof
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