CN108530056B - Giant dielectric low-loss barium strontium titanate ceramic and preparation method thereof - Google Patents
Giant dielectric low-loss barium strontium titanate ceramic and preparation method thereof Download PDFInfo
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Abstract
Disclosed is a giant dielectric low-loss barium strontium titanate ceramic with a chemical formula of Ba1‑xSrxTiO3Wherein x is the mole number of Sr and the range of x is 0<x is less than or equal to 0.3. In addition, a preparation method of the barium strontium titanate ceramic is also disclosed. The barium strontium titanate ceramic prepared by the method improves the dielectric constant of a barium titanate ceramic product, simultaneously reduces the loss of the barium titanate ceramic product, and realizes the breakthrough of a barium titanate ceramic system, thereby effectively improving the energy storage density and the comprehensive performance of the barium titanate ceramic product, expanding the application field of the barium titanate ceramic product as a high-voltage energy storage dielectric material, and greatly promoting the popularization and the application of the system material.
Description
Technical Field
The invention relates to the technical field of functional materials, in particular to giant dielectric low-loss barium strontium titanate ceramic and a preparation method thereof.
Background
With the development of science and technology, various devicesThe miniaturization and miniaturization of the devices put higher demands on the material performance, and various high dielectric and giant dielectric constant materials are developed in succession. Barium titanate (BaTiO) at room temperature3) The barium titanate ceramic is a tetragonal phase structure, is a common ferroelectric material, and has excellent dielectric properties, but the dielectric loss of the barium titanate ceramic is difficult to be greatly reduced by a common process means, so that the further development of the barium titanate material is limited. The strontium titanate ceramic at room temperature is of a cubic phase structure, has a high relative dielectric constant and low dielectric loss, and has great development potential in the years.
Barium strontium titanate is used as infinite solid solution of barium titanate and strontium titanate, and both strontium titanate and barium titanate are ABO3The perovskite structure, so barium strontium titanate has the characteristics of both the high dielectricity of barium titanate and the low loss factor of strontium titanate. Through the analysis of the unit cell structure, the Ba and Sr atoms in the specific crystal structure of the barium strontium titanate are randomly distributed in the A position of the unit cell and can be replaced in any proportion in the [ TiO ]6]The six oxygen atoms in the octahedron form relatively large voids, resulting in intermediate Ti4+A certain displacement can be carried out, and the displacement can cause the local charge distribution in the crystal to be uneven, so that spontaneous polarization is generated. This is currently one of the hot researches on ceramic dielectric materials.
The Chinese patent application (application number: 201310115238) discloses a barium strontium titanate-based dielectric temperature stable ceramic capacitor material, wherein the room temperature dielectric constant is larger than 4300, and the dielectric stability meets the X6R standard, but the loss is not involved. The Chinese patent application (application number: 201510708432.2) also discloses a sintering method of barium strontium titanate, which prepares barium titanate powder by a sol-gel method and sinters the barium titanate powder at high temperature to prepare high dielectric constant ceramics, but the method has complex process, not only needs to prepare the barium titanate powder by the sol-gel method, but also needs to sinter the barium titanate powder at high temperature by a muffle furnace, and has longer preparation period and larger energy consumption.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide barium strontium titanate ceramic (marked as giant dielectric low-loss barium strontium titanate ceramic) with high dielectric constant and lower loss, thereby effectively improving the energy storage density of ceramic products and expanding the field of the ceramic products as high-voltage energy storage dielectric materials. The invention also aims to provide a preparation method of the giant dielectric low-loss barium strontium titanate ceramic.
The invention is realized by the following technical scheme:
a barium strontium titanate ceramic with a chemical formula of Ba1-xSrxTiO3Wherein x is the mole number of Sr and the range of x is 0<x≤0.3。
As an illustrative example, the chemical formula of the barium strontium titanate ceramic of the present invention is preferably as follows: ba0.7Sr0.3TiO3、Ba0.8Sr0.2TiO3Or Ba0.9Sr0.1TiO3。
The invention provides a preparation method of the barium strontium titanate ceramic, which comprises the following steps:
(1) raw material SrCO3、BaCO3、TiO2Ball milling, mixing and drying to obtain mixed powder;
(2) the mixed powder is subjected to heat preservation to obtain barium strontium titanate powder with the chemical general formula of Ba1-xSrxTiO3Wherein x is the mole number of Sr and the range of x is 0<x≤0.3；
(3) Carrying out secondary ball milling on the barium strontium titanate powder, drying, granulating, carrying out compression molding, and carrying out cold isostatic pressing to obtain a ceramic blank;
(4) the ceramic blank is sintered after being heated and subjected to plastic removal to obtain barium strontium titanate ceramic with the chemical general formula of Ba1- xSrxTiO3Wherein x is the mole number of Sr and the range of x is 0<x≤0.3。
In the step (1), the raw material SrCO3、BaCO3、TiO2Reacting according to the chemical dose ratio to obtain barium strontium titanate powder with the chemical general formula of Ba1-xSrxTiO3Wherein x is the mole number of Sr and the range of x is 0<x is less than or equal to 0.3. Such as the raw material SrCO3、BaCO3、TiO2May be 1: 9: 10 or 2: 8: 10 or 3: 7: 10.
in the step (1), the ball milling medium used for ball milling is ethanol, and preferably absolute ethanol.
In the step (1), the ball milling is carried out by the following raw materials: ball: the mass ratio of the ball milling medium is 1: (1-2): (1-2), preferably 1: 1.2: 1.2.
in the step (1), the ball milling time is 6-18h, preferably 16 h.
In the step (2), the heat preservation temperature may be 1050-1200 ℃, and is preferably 1100 ℃.
In the step (2), the heat preservation time can be 3-6h, and is preferably 4 h.
In the step (3), the operation method of the secondary ball milling is the same as that of the ball milling in the step (1).
In the step (3), the sieving after ball milling is performed by a 100-mesh and 120-mesh sieve, preferably a 120-mesh sieve.
In the step (3), the binder used for the granulation is a 3-5wt% aqueous polyvinyl alcohol solution, and as an illustrative example, the binder used is a 4wt% aqueous polyvinyl alcohol solution.
In the step (3), the amount of the polyvinyl alcohol aqueous solution is 5-15 wt% of the weight of the barium strontium titanate powder, for example, the amount of the polyvinyl alcohol aqueous solution is 10wt% of the weight of the barium strontium titanate powder.
In the step (3), the granulation and sieving are performed by a 40-60 mesh sieve, and a 40-mesh sieve is more preferable.
In the step (3), the press forming is performed under a pressure of 15 to 20MPa, and more preferably under a pressure of 20 MPa.
In the step (3), the pressure holding time of the compression molding is 3-5min, and more preferably 5 min.
In the step (3), the pressing forming is to press a blank with the thickness of about 1.2mm and the diameter of about 12 mm.
In the step (3), the pressure of the cold isostatic pressing process is 150-200MPa, and preferably 190 MPa.
In the step (3), the pressure maintaining time of the cold isostatic pressing process is 1-3min, preferably 2 min.
And (4) heating and removing the plastic, namely placing the ceramic blank obtained in the step (3) in air, heating, then preserving the temperature, and finally naturally cooling to room temperature.
Preferably, the temperature is raised to 600-650 ℃ in the temperature-raising and plastic-removing process, and more preferably 600 ℃;
preferably, the heating rate is 1.5-2 ℃/min in the heating and plastic removing process, and further preferably 2 ℃/min;
preferably, the temperature is kept for 2-3h, and more preferably for 3h in the temperature-rising plastic-removing process.
In the step (4), the sintering temperature is 1250-.
In the step (4), the sintering time is 3-6h, and more preferably 5 h.
The invention has the following effects:
the giant dielectric low-loss barium strontium titanate ceramic formula system adopted by the invention obviously improves the dielectric constant of the ceramic product and reduces the dielectric loss, thereby effectively improving the energy storage density and the comprehensive performance of the ceramic product and expanding the field of high-voltage energy storage dielectric materials. Meanwhile, the preparation method has simple process, the adopted formula system enhances the flowability of the powder, namely accelerates the diffusion process of substances, thereby greatly reducing the sintering temperature, being easy to control the preparation, having stable and reliable quality of ceramic products and greatly promoting the popularization and application of the system material.
Drawings
FIG. 1 is an XRD spectrum of a sample of barium strontium titanate ceramics according to examples 1-3 of the present invention and comparative example 1.
FIG. 2 is a graph showing the dielectric constant spectra of barium strontium titanate ceramic samples according to examples 1 to 3 of the present invention and comparative example 1.
Fig. 3 is a dielectric loss spectrum of samples of barium strontium titanate ceramics of examples 1-3 of the present invention and comparative example 1.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Furthermore, it should be understood that various changes or modifications can be made by those skilled in the art after reading the description of the present invention, and such equivalents also fall within the scope of the invention.
Examples
TABLE 1
Based on the amounts of the raw materials in Table 1, ceramic samples, BaTiO, were obtained by the following preparation procedure3、Ba0.7Sr0.3TiO3、Ba0.8Sr0.2TiO3、Ba0.9Sr0.1TiO3The preparation method comprises the following steps:
(1) mixing SrCO3，BaCO3And TiO2Weighing the raw materials according to the dosage shown in the table 1, and mixing the raw materials in mass ratio: agate ball mill: the absolute ethyl alcohol is 1: 1.2: 1.2, ball-milling the raw materials for 16 hours, and drying to obtain mixed powder;
(2) preserving the temperature of the mixed powder obtained in the step (1) at 1100 ℃ for 4 hours to obtain barium strontium titanate powder;
(3) according to mass ratio of Ba1-xSrxTiO3Powder: agate ball mill: anhydrous ethanol ═ 1: 1.2: 1.2 ball-milling the barium strontium titanate powder for 16 hours, and drying ball-milling slurry in an air atmosphere after passing through a 120-mesh screen; then adding 0.8g of 4wt% polyvinyl alcohol aqueous solution into 1.5g of dried powder as a binder for granulation, passing the granulated powder through a 40-mesh screen, maintaining the pressure for 5min at 20MPa, and performing cold isostatic pressing at 190MPa for 2min to obtain a ceramic blank;
(4) and (4) slowly heating the ceramic blank obtained in the step (3) to 600 ℃ in the air at the heating rate of 2 ℃/min, preserving the heat at 600 ℃ for 3h, and naturally cooling to room temperature. After binder is discharged, sintering is carried out for 5 hours at 1300 ℃ to prepare BaTiO3、Ba0.7Sr0.3TiO3、Ba0.8Sr0.2TiO3、Ba0.9Sr0.1TiO3Ceramic samples.
Comparative example 1BaTiO of the invention3And barium strontium titanate ceramic samples Ba prepared in examples 1 to 30.7Sr0.3TiO3、Ba0.8Sr0.2TiO3、Ba0.9Sr0.1TiO3The XRD pattern of (A) is shown in figure 1. The results show that four ceramic samples on the XRD spectrum are basically free of impurity peaks, the sharpness and the intensity of the peaks show that the samples are completely crystallized, and all the peaks are cubic barium titanate perovskite structures.
Comparative example 1BaTiO of the invention3And barium strontium titanate ceramic samples Ba prepared in examples 1 to 30.7Sr0.3TiO3、Ba0.8Sr0.2TiO3、Ba0.9Sr0.1TiO3The dielectric constant of (A) was measured at a frequency of 100Hz-1MHz, and the test temperatures were all room temperature. The results show that Ba in the examples of the present invention0.7Sr0.3TiO3、Ba0.8Sr0.2TiO3、Ba0.9Sr0.1TiO3Dielectric constant of ceramic sample and BaTiO of comparative example 13Compared with the barium titanate ceramic material, the dielectric loss is reduced, and the technical breakthrough of the barium titanate ceramic material is realized.
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiment. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. A preparation method of barium strontium titanate ceramic is characterized by comprising the following steps:
(1) raw material SrCO3、BaCO3、TiO2Ball milling, mixing and drying to obtain mixed powder;
(2) the mixed powder is subjected to heat preservation to obtain barium strontium titanate powder with a chemical general formulaIs Ba1-xSrxTiO3Wherein x is the mole number of Sr and the range of x is 0<x≤0.3；
(3) Carrying out secondary ball milling on the barium strontium titanate powder, drying, granulating, carrying out compression molding, and carrying out cold isostatic pressing to obtain a ceramic blank;
(4) the ceramic blank is sintered after being heated and subjected to plastic removal to obtain barium strontium titanate ceramic with the chemical general formula of Ba1-xSrxTiO3Wherein x is the mole number of Sr and the range of x is 0<x≤0.3；
In the step (1), a ball milling medium used for ball milling is ethanol;
in the step (1), the ball milling is carried out by the following raw materials: ball: the mass ratio of the ball milling medium is 1: (1-2): (1-2);
in the step (1), the ball milling time is 6-18 h;
in the step (2), the heat preservation temperature is 1050-1200 ℃;
in the step (2), the heat preservation time is 3-6 h;
in the step (3), a sieving step is further included after the ball milling, and the sieving is performed by a sieve with 100 and 120 meshes;
in the step (3), a sieving step is further included after granulation, and sieving is carried out by a sieve of 40-60 meshes;
in the step (3), the adhesive used for granulation is 3-5wt% of polyvinyl alcohol aqueous solution;
in the step (3), the dosage of the polyvinyl alcohol aqueous solution is 10-15wt% of the weight of the barium strontium titanate powder;
in the step (3), the compression molding is performed under the pressure of 15-20 MPa;
in the step (3), the pressure maintaining time of the compression molding is 3-5 min;
in the step (3), the pressing forming is carried out to press the blank with the thickness of 1.2mm and the diameter of 12 mm;
in the step (3), the pressure of the cold isostatic pressing process is 150-; the pressure maintaining time of the cold isostatic pressing process is 1-3 min;
in the step (4), the heating and plastic removing step is that the ceramic blank obtained in the step (3) is placed in air, heated and then insulated, and finally naturally cooled to room temperature; heating to 600-650 ℃ in the heating and plastic removing process; the heating rate is 1.5-2 ℃/min in the heating and plastic removing process; the temperature is kept for 2-3h in the heating and plastic removing process;
in the step (4), the sintering temperature is 1250-1300 ℃;
in the step (4), the sintering time is 3-6 h.
2. The method of preparing barium strontium titanate ceramic according to claim 1, wherein in step (1), the raw material SrCO is3、BaCO3、TiO2Reacting according to the chemical dose ratio to obtain barium strontium titanate powder with the chemical general formula of Ba1-xSrxTiO3Wherein x is the mole number of Sr and the range of x is 0<x≤0.3。
3. The method of preparing a barium strontium titanate ceramic according to claim 1 or 2, wherein in step (1), the raw material SrCO is3、BaCO3、TiO2In a molar ratio of 1: 9: 10 or 2: 8: 10 or 3: 7: 10;
in the step (1), the ball milling is carried out by the following raw materials: ball: the mass ratio of the ball milling medium is 1: 1.2: 1.2;
in the step (1), the ball milling time is 16 h.
4. The method for preparing barium strontium titanate ceramic according to claim 1 or 2, wherein in the step (3), the ball-milled and sieved powder is sieved by a 120-mesh sieve;
in the step (3), the adhesive used for granulation is 4wt% of polyvinyl alcohol aqueous solution;
in the step (3), the dosage of the polyvinyl alcohol aqueous solution is Ba1-xSrxTiO310wt% of the powder;
in the step (3), sieving the granules after granulation to obtain a sieve with 40 meshes;
in the step (3), the compression molding is performed under 20 MPa;
in the step (3), the pressure maintaining time of the compression molding is 5 min;
in the step (3), the pressure of the cold isostatic pressing process is 190 MPa;
and (3) keeping the pressure of the cold isostatic pressing process for 2 min.
5. The method for preparing barium strontium titanate ceramic according to claim 1 or 2, wherein in the step (4), the temperature is raised to 600 ℃ during the temperature-raising and plastic-removing process;
in the step (4), the heating rate is 2 ℃/min in the heating and plastic removing processes;
in the step (4), heat preservation is carried out for 3 hours in the heating and plastic removing process;
in the step (4), the sintering time is 5 h.
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