CN110386815B - Barium strontium titanate composite zinc aluminate ceramic material with high adjustable rate, low loss and practicability - Google Patents

Barium strontium titanate composite zinc aluminate ceramic material with high adjustable rate, low loss and practicability Download PDF

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CN110386815B
CN110386815B CN201910667997.9A CN201910667997A CN110386815B CN 110386815 B CN110386815 B CN 110386815B CN 201910667997 A CN201910667997 A CN 201910667997A CN 110386815 B CN110386815 B CN 110386815B
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strontium titanate
barium strontium
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zinc aluminate
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张明伟
王威
沈世婷
辛乐
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Shandong University of Technology
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    • C04B35/468—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates based on barium titanates
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Abstract

The ferroelectric dielectric material of the barium strontium titanate-based composite zinc aluminate ceramic with adjustable high electricity and low loss is characterized in that the general formula of the component of the ferroelectric dielectric material of the barium strontium titanate-based composite zinc aluminate ceramic with adjustable high electricity and low loss is as follows: (1-x) Ba0.4Sr0.6TiO3‑xZnAl2O4Wherein the value range of x is more than or equal to 30 wt% and less than or equal to 70 wt%, and BaTiO is selected3Powder, SrTiO3Powder, ZnO powder and Al2O3The powder is used as main raw material according to (1-x) Ba0.4Sr0.6TiO3‑xZnAl2O4Preparing materials, ball milling, drying, pre-sintering at high temperature to prepare mixed powder, tabletting, pre-sintering at 550-600 ℃, and sintering at 1400-1450 ℃. The ferroelectric dielectric material of the high-electric adjustable low-loss barium strontium titanate-based composite zinc aluminate ceramic prepared by the invention has stable performance in a wide working temperature range and high comprehensive performance.

Description

Barium strontium titanate composite zinc aluminate ceramic material with high adjustable rate, low loss and practicability
Technical Field
The invention belongs to the technical field of electronic materials and devices, and particularly relates to a ferroelectric dielectric material of high-voltage adjustable low-loss barium strontium titanate-based composite zinc aluminate ceramic and a preparation method thereof.
Background
An important characteristic of ferroelectric materials is dielectric nonlinearity, i.e., the dielectric constant can change with a change in an applied electric field. This makes ferroelectric materials useful in microwave devices such as tunable oscillators, filters, phase shifters, and varactors. The ferroelectric material barium strontium titanate is an ideal candidate material, and has the characteristics of high tunable rate, low dielectric loss, large dielectric constant and the like. In addition, the Curie temperature can be changed by adjusting Ba/Sr to be in paraelectric phase, which is very favorable for working at room temperature. However, the barium strontium titanate ceramic has the problem that the high dielectric constant is difficult to meet the requirements of impedance matching and high power between the barium strontium titanate ceramic and an excitation source, which limits the application of the barium strontium titanate ceramic in the field of microwave tunable devices. The tunability has a strong electric field dependence and can be expressed as Tunability (abbreviated as T) = [ ]ε r(0)–ε r(E) ] /ε r(0)X 100%, whereinε r(0)、ε r(E) The dielectric constants are respectively under a zero electric field and an external direct current electric field. For example, in a typical applied phase shifter, the ability of the device to change phase angle is largely dependent on the tunability of the materialAnd if the dielectric loss is too large, the device can generate heat seriously, so that a high-power low-loss adjustable material is needed. In the performance tailoring of materials, the tunable rate, the dielectric loss and the dielectric constant are often in a mutual restriction relationship, so that the existing research work is to compromise and regulate the parameters of the tunable rate, the dielectric loss and the dielectric constant so as to obtain the optimal performance of a device. The dielectric material and the ferroelectric material are always the simplest and most effective methods, and researchers find that the dielectric constant of the ferroelectric material can be diluted by compounding the low-loss linear dielectric material, so that the dielectric loss of the material is reduced; the tunability of the composite material is impaired in relation to the dilution of the ferroelectricity of the ferroelectric material and the redistribution of the electric field caused by the linear dielectric material under the electric field. Ferroelectric dielectric systems have been reported, such as BST-MgAl2O4、BST-Mg2TiO4The dielectric constant, dielectric loss and dielectric tunability have met practical requirements, but the problems of too low Q value (reciprocal of dielectric loss) and insufficiently high tunability under microwave still exist, and further improvement of the overall performance is still needed.
Disclosure of Invention
The invention aims to provide a high-power adjustable low-loss barium strontium titanate-based composite zinc aluminate ferroelectric dielectric ceramic material with high comprehensive performance and simple preparation process, which has the technical scheme that:
the ferroelectric dielectric material of the high-electricity adjustable low-loss barium strontium titanate-based composite zinc aluminate ceramic is characterized in that the chemical composition formula of the ferroelectric dielectric material of the high-electricity adjustable low-loss barium strontium titanate-based composite zinc aluminate ceramic is as follows: (1-x) Ba0.4Sr0.6TiO3-xZnAl2O4Wherein the value range of x is more than or equal to 30 wt% and less than or equal to 70 wt%, and the preparation method comprises the following steps:
(1) selecting BaTiO3Powder, SrTiO3Powder, ZnO powder and Al2O3The powder is used as main raw material according to (1-x) Ba0.4Sr0.6TiO3-xZnAl2O4Proportioning the Ba, Sr, Ti, Zn and Al according to the stoichiometric ratioThe raw materials are placed in a nylon ball milling tank, zirconia balls and ball milling media are added for ball milling, and after discharging and drying, pre-sintering and grinding are carried out to obtain mixed powder 1; the temperature for pre-sintering is 1100-1200 ℃, and the sintering time is 4-6 hours.
(2) Adding the mixed powder 1 in the step (1) into zirconia balls and absolute ethyl alcohol or deionized water for ball milling for 24-48 hours, discharging, drying and sieving to obtain mixed powder 2;
(3) adding the mixed powder 2 in the step (2) into a polyvinyl alcohol aqueous solution with the mass ratio of 7-10%, uniformly mixing, granulating, and pressing under the pressure of 10-100 MPa to prepare a ceramic green sheet;
(4) carrying out glue discharging treatment on the ceramic green sheet in the step (3) at the temperature of 550-600 ℃ for 4-10 hours; and after the binder is removed, sintering the mixture at 1400-1450 ℃ for 4-6 hours to form ceramic, thus obtaining the ferroelectric dielectric material of the high-electricity adjustable low-loss barium strontium titanate-based composite zinc aluminate ceramic.
The high-electricity adjustable low-loss barium strontium titanate-based composite zinc aluminate ferroelectric dielectric ceramic material has the following advantages:
(1) the Curie temperature of the composite ceramic is controlled in a proper range through the preferable Ba/Sr, and the composite ceramic is (1-x) Ba0.4Sr0.6TiO3-xZnAl2O4The dielectric property can be adjusted in a wide working temperature range, and the method is particularly suitable for working temperatures of room temperature and above;
(2) the dielectric constant is adjusted in different suitable intervals by using different x mass ratios, so that the requirements of different devices under application can be met, and the application range of the material is widened;
(3) the dielectric constant is low, the dielectric loss is low, the electrical adjustability is high (when the mass percentage of the array adjusting components of x is changed, the high performance of the three components can be met at the same time), and the comprehensive dielectric performance under microwave is high;
(4) the traditional electronic ceramic preparation process is adopted, so that the process is simple; the material system belongs to green environment-friendly materials, and has no toxic or side effect. The material has excellent performance and is suitable for components such as a microwave adjustable oscillator, a filter, a phase shifter, a microwave dielectric antenna and the like.
Detailed Description
Example 1
(1) According to 70 wt% of Ba0.4Sr0.6TiO3+30 wt % ZnAl2O4In the chemical ratio of BaTiO38.4g、SrTiO312.6g, ZnO4g and Al2O35g of powder, namely placing the prepared raw materials into a nylon ball milling tank, adding zirconia balls and a ball milling medium, carrying out ball milling, discharging, drying, pre-sintering and grinding to obtain mixed powder 1; the pre-sintering temperature is 1100 ℃ and 1200 ℃, and the sintering time is 4 hours;
(2) adding zirconia balls and absolute ethyl alcohol or deionized water into the mixed powder 1 in the step (1) to perform ball milling for 24 hours, discharging, drying and sieving to obtain mixed powder 2;
(3) adding the mixed powder 2 in the step (2) into a polyvinyl alcohol aqueous solution with the mass ratio of 10%, uniformly mixing and granulating, and then pressing under the pressure of 10MPa to prepare a ceramic green sheet;
(4) carrying out heat preservation on the ceramic green sheet in the step (3) at 550 ℃ for 10 hours to carry out glue discharging treatment; after the binder is removed, the ceramic is sintered for 4 hours at 1450 ℃, and the ferroelectric dielectric material of the barium strontium titanate-based composite zinc aluminate ceramic with high electricity, adjustable and low loss is prepared.
BaTiO used for experiment3Purity of 99.5%, produced by Michelin Biochemical technology Ltd, SrTiO399.5% purity, Michelin Biochemical technology Ltd, 99.9% purity ZnO, Tianjin chemical reagent III, Al2O3The purity is 99.9 percent, and the product is produced by chemical reagents of national drug group. The performance parameters of the ferroelectric dielectric material of the prepared high-electric adjustable low-loss barium strontium titanate-based composite zinc aluminate ceramic are shown in Table 1.
Example 2
(1) According to 50 wt% of Ba0.4Sr0.6TiO3+50 wt % ZnAl2O4In the chemical ratio of BaTiO37.0g、SrTiO39.0g, ZnO6.7g and Al2O38.3g of powder, putting the prepared raw materials into a nylon ball milling tank, adding zirconia balls and a ball milling medium, carrying out ball milling, discharging, drying, pre-sintering and grinding to obtain mixed powder 1; the temperature for pre-sintering is 1100 ℃ and 1200 ℃ respectively, and the sintering time is 6 hours;
(2) adding zirconia balls and absolute ethyl alcohol or deionized water into the mixed powder 1 in the step (1) to perform ball milling for 30 hours, discharging, drying and sieving to obtain mixed powder 2;
(3) adding the mixed powder 2 in the step (2) into a polyvinyl alcohol aqueous solution with the mass ratio of 8%, uniformly mixing and granulating, and then pressing under the pressure of 30MPa to prepare a ceramic green sheet;
(4) carrying out heat preservation on the ceramic green sheet in the step (3) at 580 ℃ for 7 hours to carry out glue discharging treatment; after the binder is removed, the ceramic is sintered at 1400 ℃ for 6 hours to obtain the ferroelectric dielectric material of the high-electricity adjustable low-loss barium strontium titanate-based composite zinc aluminate ceramic.
BaTiO used for experiment3Purity of 99.5%, produced by Michelin Biochemical technology Ltd, SrTiO399.5% purity, Michelin Biochemical technology Ltd, 99.9% purity ZnO, Tianjin chemical reagent III, Al2O3The purity is 99.9 percent, and the product is produced by chemical reagents of national drug group. The performance parameters of the ferroelectric dielectric material of the prepared high-electric adjustable low-loss barium strontium titanate-based composite zinc aluminate ceramic are shown in Table 1.
Example 3
(1) According to 30 wt% of Ba0.4Sr0.6TiO3+70 wt % ZnAl2O4In the chemical ratio of BaTiO33.6g、SrTiO35.4g, ZnO9.3g and Al2O311.7g of powder, putting the prepared raw materials into a nylon ball milling tank, adding zirconia balls and a ball milling medium, carrying out ball milling, discharging, drying, pre-sintering and grinding to obtain mixed powder 1; the pre-sintering temperature is 1200 ℃ and 1200 ℃ respectively, and the sintering time is 5 hours;
(2) adding zirconia balls and absolute ethyl alcohol or deionized water into the mixed powder 1 in the step (1) to perform ball milling for 48 hours, discharging, drying and sieving to obtain mixed powder 2;
(3) adding the mixed powder 2 in the step (2) into a 7% polyvinyl alcohol aqueous solution by mass ratio, uniformly mixing, granulating, and pressing under the pressure of 100MPa to prepare a ceramic green sheet;
(4) carrying out heat preservation on the ceramic green sheet in the step (3) at the temperature of 600 ℃ for 4 hours to carry out glue discharging treatment; after the binder is removed, the ceramic is sintered at 1450 ℃ for 5 hours to obtain the ferroelectric dielectric material of the high-electricity adjustable low-loss barium strontium titanate-based composite zinc aluminate ceramic.
BaTiO used for experiment3Purity of 99.5%, produced by Michelin Biochemical technology Ltd, SrTiO399.5% purity, Michelin Biochemical technology Ltd, 99.9% purity ZnO, Tianjin chemical reagent III, Al2O3The purity is 99.9 percent, and the product is produced by chemical reagents of national drug group. The performance parameters of the ferroelectric dielectric material of the prepared high-electric adjustable low-loss barium strontium titanate-based composite zinc aluminate ceramic are shown in Table 1.
TABLE 1 (1-x) Ba in different compounding amounts and different firing regimes0.4Sr0.6TiO3-xZnAl2O4Electrical properties of the composite material
Figure 659435DEST_PATH_IMAGE002
The dielectric parameters of the composite material measured by the table show that the composite system has high comprehensive performance: the composite material has high adjustable rate and good stability (the adjustable rate is not weakened even if the dielectric constant is greatly reduced); the dielectric constant is regulated to a proper value, so that the requirements of different microwave devices can be met, and the Q value under microwave is kept to a better degree. For example at 30 wt% Ba0.4Sr0.6TiO3+70 wt % ZnAl2O4The dielectric constant is regulated to 178, the dielectric loss is 0.0093, the adjustability is up to 31.5 percent, and the microwave content is regulated to be higher than that of the productThe lower Q value reaches 707. The invention has simple preparation process, good repetition rate and high yield, is suitable for various microwave adjustable components and is suitable for large-scale production of enterprises.

Claims (1)

1. The ferroelectric dielectric material of the high-electricity adjustable low-loss barium strontium titanate-based composite zinc aluminate ceramic is characterized in that the chemical composition formula of the ferroelectric dielectric material of the high-electricity adjustable low-loss barium strontium titanate-based composite zinc aluminate ceramic is as follows: (1-x) Ba0.4Sr0.6TiO3-xZnAl2O4Wherein the value range of x is more than or equal to 30 wt% and less than or equal to 70 wt%, and the preparation method comprises the following steps:
(1) Selecting BaTiO3Powder, SrTiO3Powder, ZnO powder and Al2O3The powder is used as main raw material according to (1-x) Ba0.4Sr0.6TiO3-xZnAl2O4Proportioning the Ba, Sr, Ti, Zn and Al according to the stoichiometric ratio, putting the proportioned raw materials into a nylon ball milling tank, adding zirconia balls and ball milling media, carrying out ball milling, discharging, drying, presintering and grinding to obtain mixed powder 1; the temperature for pre-sintering is 1100-1200 ℃, and the sintering time is 4-6 hours;
(2) Adding the mixed powder 1 in the step (1) into zirconia balls and absolute ethyl alcohol or deionized water for ball milling for 24-48 hours, discharging, drying and sieving to obtain mixed powder 2;
(3) Adding the mixed powder 2 in the step (2) into a polyvinyl alcohol aqueous solution with the mass ratio of 7-10%, uniformly mixing, granulating, and pressing under the pressure of 10-100 MPa to prepare a ceramic green sheet;
(4) Carrying out glue discharging treatment on the ceramic green sheet in the step (3) at the temperature of 550-600 ℃ for 4-10 hours; and after the binder is removed, sintering the mixture at 1400-1450 ℃ for 4-6 hours to form ceramic, thus obtaining the ferroelectric dielectric material of the high-electricity adjustable low-loss barium strontium titanate-based composite zinc aluminate ceramic.
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