CN110668814A - Microwave dielectric material with near-zero temperature coefficient of resonant frequency - Google Patents
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Abstract
The invention discloses a microwave dielectric material with a near-zero resonant frequency temperature coefficient, which is prepared from TiO2、ZnO、Nb2O5、ZrO2As a raw material, the expression of the target composition is (Zr)1‑xTix)1‑y(Zn1/ 3Nb2/3)yO2Wherein x is 0.6-0.7, and y is 0.1-0.3. Firstly, raw materials are proportioned according to a stoichiometric formula, are presintered at 1050 ℃ after ball milling, drying and sieving, and are granulated and pressed into green bodies after ball milling and drying; heating the green body to 1250 ℃ at the speed of 5 ℃/min, preserving heat for 30 minutes, cooling to 1150 ℃ at the speed of 10 ℃/min, preserving heat for 12 hours, and cooling to obtain the resonanceThe microwave dielectric material has a frequency temperature coefficient close to zero. The two-stage sintering of the invention firstly heats the ceramic green body to a higher temperature and preserves the temperature for a short time, and then preserves the temperature for a long time at a lower temperature, so that the ceramic achieves higher density, simultaneously reduces the residual stress between two phases, and effectively improves the defect of lower Qf value of the two-phase composite microwave dielectric ceramic material.
Description
Technical Field
The present invention belongs to a ceramic composition characterized by that it is a medium-temp. sintered (Zr) with high dielectric constant and near-zero temp. coefficient of resonance frequency1-xTix)1-y(Zn1/3Nb2/3)yO2Wherein x is 0.6-0.7, and y is 0.1-0.3 series microwave dielectric ceramics and its preparation method.
Background
Microwave technology is one of the great achievements of recent scientific development. Because microwaves have the advantages of short wavelength, high frequency and the like, the microwaves have good frequency selection characteristics and are widely applied to the fields of mobile communication, satellite communication, military radar, Global Positioning System (GPS), Bluetooth technology, wireless local area network and the like. The development of microwave communication technology places new demands on the performance (sensitivity, signal-to-noise ratio, coverage, communication capacity, etc.) and size of microwave devices. Driven by this technical background, microwave dielectric ceramic materials with high dielectric constant, low dielectric loss and temperature coefficient of near-zero resonant frequency are urgently needed.
(Zr1-xTix)1-y(Zn1/3Nb2/3)yO2The microwave dielectric ceramic is a manganese-tantalum ore-rutile two-phase composite structure, the system has a high dielectric constant (40-50), a near-zero temperature coefficient and a moderate sintering temperature (1200 ℃), but the material system has a low Qf value due to the existence of residual stress between two phases, and further development of the system is limited.
Disclosure of Invention
The purpose of the invention is to overcome (Zr)1-xTix)1-y(Zn1/3Nb2/3)yO2The microwave dielectric ceramic has the defect of low Qf value due to the existence of residual stress between two phases. By adopting a two-stage sintering technology, a series of microwave dielectric ceramics with near-zero resonant frequency temperature coefficient and high quality factor are obtained, and (Zr) is provided at the same time1-xTix)1-y(Zn1/3Nb2/3)yO2Composition of microwave dielectric ceramicFormulation and process for preparing the dielectric ceramic.
The invention is realized by the following technical scheme.
A microwave dielectric material with near-zero temperature coefficient of resonance frequency, which is TiO2、ZnO、Nb2O5、ZrO2As a raw material, the expression of the target composition is (Zr)1-xTix)1-y(Zn1/3Nb2/3)yO2Wherein x is 0.6-0.7, and y is 0.1-0.3;
the preparation method of the microwave dielectric material comprises the following implementation steps:
(1) adding TiO into the mixture2、ZnO、Nb2O5、ZrO2In stoichiometric formula (Zr)1-xTix)1-y(Zn1/3Nb2/3)yO2Mixing x is 0.6-0.7 and y is 0.1-0.3, putting the powder into a polyester tank, adding deionized water and zirconium balls, and performing ball milling for 4-8 hours;
(2) putting the ball-milled raw materials in the step (1) into a drying oven, drying at 80-120 ℃ respectively, and then sieving with a 40-mesh sieve;
(3) putting the powder sieved in the step (2) into a medium-temperature furnace, presintering at 1050 ℃, preserving heat for 2-8 hours, and then sieving by a 40-mesh sieve;
(4) putting the powder subjected to the pre-sintering in the step (3) into a ball milling tank, adding zirconia balls and deionized water, and carrying out ball milling for 9-12 hours;
(5) putting the ball-milled raw materials in the step (4) into a drying oven, drying, adding 5% polyvinyl alcohol aqueous solution as an adhesive, granulating, sieving with a 80-mesh sieve, and pressing into a green body by using a powder tablet press at a pressure of 4-8 MPa;
(6) and (3) putting the green body obtained in the step (5) into a medium temperature furnace, heating to 1250 ℃ at the speed of 5 ℃/min, preserving the temperature for 30 minutes, then cooling to 1150 ℃ at the speed of 10 ℃/min, preserving the temperature for 12 hours at 1150 ℃, and then cooling along with the furnace to obtain the microwave dielectric material with the resonant frequency temperature coefficient close to zero.
And (2) ball milling is carried out in the step (1) by adopting a planetary ball mill, and the rotating speed of the ball mill is 400 r/min.
The diameter of the green body obtained in the step (5) is 10mm, and the thickness of the green body is 5 mm.
And the step (6) is sintering in an air atmosphere.
The invention provides a series of formula compositions with near-zero temperature coefficient of resonance frequency, which have higher dielectric constant, higher Qf value and lower sintering temperature and can meet the requirements of practical engineering application on microwave dielectric materials. Meanwhile, the invention also provides a novel sintering technology suitable for the two-phase composite microwave dielectric ceramic material: two-stage sintering technique. The two-section sintering is that firstly, the ceramic green body is heated to a higher temperature and is insulated for a short time, so that the green body achieves a proper density; and then the ceramic is kept at a lower temperature for a long time, so that the ceramic can reach higher density, and the residual stress between the two phases is reduced as much as possible. The method effectively overcomes the defect of low Qf value of the two-phase composite microwave dielectric ceramic material.
Detailed Description
Example 1
The invention uses TiO with purity of more than 99 percent2(analytically pure), ZnO (analytically pure), Nb2O5(analytical grade), ZrO2(analytically pure) is used as an initial raw material, and the microwave dielectric material is prepared by a solid phase method. The specific implementation steps are as follows:
(1) adding TiO into the mixture2、ZnO、Nb2O5、ZrO2In stoichiometric formula (Zr)0.4Ti0.6)0.8(Zn1/3Nb2/3)0.2O2The materials are prepared, and the powder ratio is as follows: 7.8862gZrO2、3.5086gNb2O5、7.6672gTiO2、1.1072gZnO2. Putting the powder into a polyester tank, adding 200ml of deionized water and 150g of zirconium balls, and performing ball milling for 6 hours at the rotating speed of 400 revolutions per minute;
(2) putting the ball-milled raw materials in the step (1) into a drying oven, drying at 100 ℃, and then sieving by a 40-mesh sieve;
(3) putting the dried and sieved powder in the step (2) into a medium-temperature furnace, presintering at 1050 ℃, preserving heat for 4 hours, and then sieving by a 40-mesh sieve;
(4) putting the calcined powder in the step (3) into a ball milling tank, adding 200ml of deionized water and 150g of zirconia balls, and carrying out ball milling for 12 hours at the rotating speed of 400 r/m;
(5) putting the ball-milled raw materials in the step (4) into a drying oven, drying, adding 5% polyvinyl alcohol aqueous solution as an adhesive, granulating, sieving with a 80-mesh sieve, and pressing into a green body by using a powder tablet press under the pressure of 4 MPa;
(6) and (3) putting the green body obtained in the step (5) into a medium temperature furnace, heating to 1250 ℃ at the speed of 5 ℃/min in the air atmosphere, preserving the heat for 30 minutes, then cooling to 1150 ℃ at the speed of 10 ℃/min, preserving the heat for 12 hours at 1150 ℃, and then cooling along with the furnace to obtain the microwave dielectric material with the resonant frequency temperature coefficient close to zero.
(7) The microwave dielectric property of the obtained sample, epsilon, is tested by a network analyzerr＝41.56，Qf＝46543GHz，τf＝-7.5ppm℃-1。
Example 2
The invention uses TiO with purity of more than 99 percent2(analytically pure), ZnO (analytically pure), Nb2O5And (analytically pure) and ZrO2 (analytically pure) are used as initial raw materials, and the microwave dielectric material is prepared by a solid-phase method. The specific implementation steps are as follows:
(1) adding TiO into the mixture2、ZnO、Nb2O5、ZrO2In stoichiometric formula (Zr)0.4Ti0.6)0.8(Zn1/3Nb2/3)0.2O2The materials are prepared, and the powder ratio is as follows: 6.9004gZrO2、3.5086gNb2O5、8.3060gTiO2、1.1072gZnO2. Putting the powder into a polyester tank, adding 200ml of deionized water and 150g of zirconium balls, and performing ball milling for 6 hours at the rotating speed of 400 revolutions per minute;
(2) putting the ball-milled raw materials in the step (1) into a drying oven, drying at 100 ℃, and then sieving by a 40-mesh sieve;
(3) putting the dried and sieved powder in the step (2) into a medium-temperature furnace, presintering at 1050 ℃, preserving heat for 4 hours, and then sieving by a 40-mesh sieve;
(4) putting the calcined powder in the step (3) into a ball milling tank, adding 200ml of deionized water and 150g of zirconia balls, and carrying out ball milling for 12 hours at the rotating speed of 400 r/m;
(5) putting the ball-milled raw materials in the step (4) into a drying oven, drying, adding 5% polyvinyl alcohol aqueous solution as an adhesive, granulating, sieving with a 80-mesh sieve, and pressing into a green body by using a powder tablet press under the pressure of 4 MPa;
(6) and (3) putting the green body obtained in the step (5) into a medium temperature furnace, heating to 1250 ℃ at the speed of 5 ℃/min in the air atmosphere, preserving the heat for 30 minutes, then cooling to 1150 ℃ at the speed of 10 ℃/min, preserving the heat for 12 hours at 1150 ℃, and then cooling along with the furnace to obtain the microwave dielectric material with the resonant frequency temperature coefficient close to zero.
(7) The microwave dielectric property of the obtained sample, epsilon, is tested by a network analyzerr＝44.64，Qf＝42772GHz，τf＝+1.1ppm℃-1。
Examples 3 to 9
Except the value ranges of x and y, other process parameters of the embodiments 3-9 are completely the same as those of the above embodiments, and the main parameters and the microwave dielectric properties of the specific embodiments are detailed in table 1.
TABLE 1
Claims (4)
1. A microwave dielectric material with near-zero temperature coefficient of resonance frequency, which is TiO2、ZnO、Nb2O5、ZrO2As a raw material, the expression of the target composition is (Zr)1-xTix)1-y(Zn1/3Nb2/3)yO2Wherein x is 0.6-0.7, and y is 0.1-0.3.
The preparation method of the microwave dielectric material comprises the following implementation steps:
(1) adding TiO into the mixture2、ZnO、Nb2O5、ZrO2In stoichiometric formula (Zr)1-xTix)1-y(Zn1/3Nb2/3)yO2Mixing the powder materials, wherein x is 0.6-0.7 and y is 0.1-0.3Adding deionized water and zirconium balls into a polyester tank, and performing ball milling for 4-8 hours;
(2) putting the ball-milled raw materials in the step (1) into a drying oven, drying at 80-120 ℃ respectively, and then sieving with a 40-mesh sieve;
(3) putting the powder sieved in the step (2) into a medium-temperature furnace, presintering at 1050 ℃, preserving heat for 2-8 hours, and then sieving by a 40-mesh sieve;
(4) putting the powder subjected to the pre-sintering in the step (3) into a ball milling tank, adding zirconia balls and deionized water, and carrying out ball milling for 9-12 hours;
(5) putting the ball-milled raw materials in the step (4) into a drying oven, drying, adding 5% polyvinyl alcohol aqueous solution as an adhesive, granulating, sieving with a 80-mesh sieve, and pressing into a green body by using a powder tablet press at a pressure of 4-8 MPa;
(6) and (3) putting the green body obtained in the step (5) into a medium temperature furnace, heating to 1250 ℃ at the speed of 5 ℃/min, preserving the temperature for 30 minutes, then cooling to 1150 ℃ at the speed of 10 ℃/min, preserving the temperature for 12 hours at 1150 ℃, and then cooling along with the furnace to obtain the microwave dielectric material with the resonant frequency temperature coefficient close to zero.
2. A microwave dielectric material with a resonant frequency temperature coefficient close to zero as claimed in claim 1, wherein said step (1) is performed by ball milling with a planetary ball mill, and the rotation speed of the ball mill is 400 rpm.
3. A microwave dielectric material with a temperature coefficient of resonance frequency close to zero as claimed in claim 1, wherein the green compact of step (5) has a diameter of 10mm and a thickness of 5 mm.
4. A microwave dielectric material with a temperature coefficient of resonance frequency close to zero as claimed in claim 1, wherein said step (6) is sintering in air atmosphere.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113880573A (en) * | 2021-09-10 | 2022-01-04 | 天津大学 | Temperature-stable low-dielectric-loss microwave dielectric ceramic material and preparation method thereof |
| CN114349501A (en) * | 2022-01-28 | 2022-04-15 | 郑州轻工业大学 | ZYTO system composite ceramic material and preparation method thereof |
| CN115925415A (en) * | 2022-10-26 | 2023-04-07 | 云南银峰新材料有限公司 | Ion-modified microwave dielectric ceramic, preparation method thereof and microwave component |
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