CN111635230A - High-quality-factor strontium cerate microwave dielectric ceramic material and preparation method thereof - Google Patents

High-quality-factor strontium cerate microwave dielectric ceramic material and preparation method thereof Download PDF

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CN111635230A
CN111635230A CN202010466867.1A CN202010466867A CN111635230A CN 111635230 A CN111635230 A CN 111635230A CN 202010466867 A CN202010466867 A CN 202010466867A CN 111635230 A CN111635230 A CN 111635230A
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张启龙
周富明
王浩
杨辉
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Zhejiang University ZJU
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Abstract

The invention relates to the field of material science, and aims to provide a strontium cerate microwave dielectric ceramic material with a high quality factor and a preparation method thereof. Is prepared from the ceramic base material Sr2CeO4Middle doped composite assistant Li2CO3‑Bi2O3Reducing the sintering temperature to 875-1100 ℃; the chemical expression of the dielectric ceramic material is as follows: (100-a) wt% Sr2CeO4+a wt％Li2CO3‑Bi2O3(ii) a Wherein 0 < a < 4, Li2CO3:Bi2O3The mass ratio of (a) to (b) is 0.25 to 4. The invention is realized by reducing Sr2CeO4The sintering temperature of the ceramic avoids the abnormal growth of ceramic crystal grains, and maintains the structural stability and excellent microwave dielectric property of the ceramic crystal. The invention has simple preparation process, low cost and good repeatability, is suitable for large-scale production, and has wide application prospect in the fields of microwave components such as filters, antennas, dielectric substrates and the like.

Description

High-quality-factor strontium cerate microwave dielectric ceramic material and preparation method thereof
Technical Field
The invention belongs to the field of material science, and particularly relates to a high-quality-factor microwave dielectric ceramic material and a preparation method thereof.
Background
In recent years, it has become possible to provide,with the rapid development of 5G mobile communication, satellite communication, wireless network, Bluetooth and other technologies, microwave devices are developing beyond the direction of miniaturization, high frequency and light weight, and higher requirements are put forward on microwave dielectric ceramic materials, namely, the dielectric constant is serialized to meet the requirements of different communication frequency bands, the higher the quality factor Q × f is, the better the quality factor Q × f is, the lower the sintering temperature is, the better the microstructure control and energy conservation are facilitated, the frequency temperature coefficient is controllable and adjustable, and the strontium cerate Sr is2CeO4Has extremely high quality factor and moderate dielectric constant, and attracts wide attention. But has the disadvantages that the strontium cerate system has high sintering temperature (1400 ℃), and the crystal phase structure is unstable, thereby limiting the practical application of the strontium cerate system.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects of the existing material system and technology and providing a high-quality-factor microwave dielectric ceramic material with low sintering temperature and stable crystalline phase structure and a preparation method thereof.
In order to solve the technical problem, the solution provided by the invention is as follows:
the high-quality factor strontium cerate microwave dielectric ceramic material is prepared by doping a composite auxiliary agent in a ceramic base material to reduce the sintering temperature to 875-1100 ℃; wherein the chemical formula of the ceramic base material is Sr2CeO4The chemical formula of the composite auxiliary agent is Li2CO3-Bi2O3(ii) a The chemical expression of the dielectric ceramic material is as follows:
(100-a)wt％Sr2CeO4+a wt％Li2CO3-Bi2O3
wherein 0 < a < 4, Li2CO3:Bi2O3The mass ratio of (a) to (b) is 0.25 to 4.
The invention further provides a preparation method of the dielectric ceramic material, which comprises the following steps:
(1) according to SrCO3:CeO2The raw material SrCO is weighed according to the molar ratio of 2:13And CeO2Powder is subjected to ball milling and mixing for 4 hours; pre-burning for 4h at 1150 ℃, and performing secondary ball milling to obtain Sr2CeO4A ceramic base material;
(2) according to Sr2CeO4With Li2CO3-Bi2O3A, Li in a mass ratio of (100-a)2CO3-Bi2O3Li in (1)2CO3And Bi2O3Taking raw material Li with the mass ratio of x to y being 0.25-42CO3And Bi2O3Powder; sr is2CeO4Ceramic base material, Li2CO3And Bi2O3Ball milling and mixing the powder, and then drying;
(3) adding the mixed powder prepared in the step (2) into a polyvinyl alcohol solution, and uniformly mixing; pressing under the pressure of 120MPa to prepare a cylindrical blank;
(4) and (4) sintering the blank obtained in the step (3) for 4 hours at the temperature of 875-.
In the invention, in the step (1), the ball milling and mixing are carried out under the condition of ethanol infiltration.
In the invention, in the step (3), the mass fraction of the polyvinyl alcohol solution is 15%, and the mass percentage of the mixed powder in the polyvinyl alcohol solution is 8%.
Compared with the prior art, the invention has the beneficial effects that:
1. in the microwave dielectric ceramic of the invention, strontium cerate Sr has high Q × f value2CeO4Is a ceramic base material, by doping with Li2CO3-Bi2O3Composite assistants of Li in sintering process2CO3And Bi2O3Liquid phase is generated, ceramic particles are infiltrated, the sintering mass transfer process is promoted, and the Sr is obviously reduced2CeO4The sintering temperature of the ceramic. Pure Sr2CeO4The sintering temperature range is 1300-1400 ℃; the invention is based on the addition of Li2CO3-Bi2O3The sintering temperature range is reduced to 875-1100 ℃.
2. The invention is realized by reducing Sr2CeO4The sintering temperature of the ceramic is controlled to avoid the abnormal growth of ceramic grainsThe microwave dielectric ceramic material has dielectric constant of 13.5-14.5, Q × f value of 69000-100000GHz, and frequency temperature coefficient of-60 ppm/deg.C to-70 ppm/deg.C.
3. The invention has simple preparation process, low cost and good repeatability, is suitable for large-scale production, and has wide application prospect in the fields of microwave components such as filters, antennas, dielectric substrates and the like.
Detailed Description
The following examples are presented to enable those skilled in the art to more fully understand the present invention and are not intended to limit the invention in any way.
Examples
1. According to molar ratio SrCO3:CeO2Weighing SrCO as raw material 2:13And CeO2Ball milling and mixing materials for 4 hours under the condition of ethanol infiltration; baking, pre-sintering at 1150 deg.C for 4 hr to obtain Sr2CeO4And (5) standby.
2. According to the total mass ratio of Sr2CeO4:Li2CO3-Bi2O3A starting materials were prepared with different Li2CO3-Bi2O3Ingredients the chemical formula of the total ingredients can be written as:
P0.5-1 99.5wt％Sr2CeO4-0.4wt％Bi2O3-0.1wt％Li2CO3；(a＝0.5,x:y＝4)
P0.5-2 99.5wt％Sr2CeO4-0.3wt％Bi2O3-0.2wt％Li2CO3；(a＝0.5,x:y＝1.5)
P0.5-3 99.5wt％Sr2CeO4-0.2wt％Bi2O3-0.3wt％Li2CO3；(a＝0.5,x:y＝0.67)
P0.5-4 99.5wt％Sr2CeO4-0.1wt％Bi2O3-0.4wt％Li2CO3；(a＝0.5,x:y＝0.25)
P1-1 99wt％Sr2CeO4-0.8wt％Bi2O3-0.2wt％Li2CO3；(a＝1,x:y＝4)
P1-2 99wt％Sr2CeO4-0.6wt％Bi2O3-0.4wt％Li2CO3；(a＝1,x:y＝1.5)
P1-3 99wt％Sr2CeO4-0.4wt％Bi2O3-0.6wt％Li2CO3；(a＝1,x:y＝0.67)
P1-4 99wt％Sr2CeO4-0.2wt％Bi2O3-0.8wt％Li2CO3；(a＝1,x:y＝0.25)
P4-1 96wt％Sr2CeO4-3.2wt％Bi2O3-0.8wt％Li2CO3；(a＝4,x:y＝4)
P4-2 96wt％Sr2CeO4-2.4wt％Bi2O3-1.6wt％Li2CO3；(a＝4,x:y＝1.5)
P4-3 96wt％Sr2CeO4-1.6wt％Bi2O3-2.4wt％Li2CO3；(a＝4,x:y＝0.67)
P4-4 96wt％Sr2CeO4-0.8wt％Bi2O3-3.2wt％Li2CO3；(a＝4,x:y＝0.25)
3. adding the prepared P0.5-P4 mixed powder into 15% polyvinyl alcohol solution by mass percent according to the mass percent of 8 wt%, uniformly mixing, and performing compression molding under the pressure of 120MPa to prepare a cylindrical blank.
4. And sintering the blank at 875-1100 ℃ for 4h to obtain the strontium cerate microwave dielectric ceramic with high quality factor.
Comparative example
According to SrCO3:CeO2The raw material SrCO is weighed according to the molar ratio of 2:13And CeO2Ball-milling the powder, mixing for 4h, presintering at 1150 ℃ for 4h to obtain pure Sr2CeO4Powder material; pure Sr2CeO4Adding the powder into 15 percent polyvinyl alcohol solution according to the mass percentage of 8 percent by weight, uniformly mixing, and performing stirring under the pressure of 120MPaPerforming compression molding to prepare a cylindrical blank; sintering the blank at 1300 plus 1400 ℃ for 4h to obtain pure Sr2CeO4Microwave dielectric ceramics.
Performance testing
Aiming at pure Sr without addition2CeO4And the product of the invention is used for microwave dielectric property test.
The test instrument is an Agilent E5071C network analyzer, the test conditions of dielectric constant and Q × f value are 25 ℃, 9-10GHz, the test temperature range of frequency temperature coefficient is 25-80 ℃, and no added pure Sr2CeO4And the microwave dielectric properties of the product of the invention are shown in tables 1 and 2, respectively.
TABLE 1 pure Sr2CeO4Microwave dielectric properties at different sintering temperatures
Figure BDA0002512951150000031
TABLE 2 microwave dielectric Properties of P0.5-P4 groups at different sintering temperatures
Figure BDA0002512951150000041
As can be seen from the data in tables 1 and 2, the vector Sr2CeO4In which a composite assistant Li is added2CO3-Bi2O3When the sintering temperature of the a-1 group and the sintering temperature of the P1-1 group is 1075 ℃, the maximum Q × f value of the material is more than 100,000GHz, and the sintering temperature is obviously reduced along with Li in the composite auxiliary agent2CO3The content is gradually increased, the temperature is further reduced, and the ceramics of P1-3 group and P1-4 group can be sintered at the temperature below 950 ℃ and have excellent Q × f value which is more than 65,000 GHz.

Claims (4)

1. The high quality factor strontium cerate microwave dielectric ceramic material is characterized by that it is in ceramic base materialDoping a composite auxiliary agent to reduce the sintering temperature to 875-1100 ℃; wherein the chemical formula of the ceramic base material is Sr2CeO4The chemical formula of the composite auxiliary agent is Li2CO3-Bi2O3(ii) a The chemical expression of the dielectric ceramic material is as follows:
(100-a)wt％Sr2CeO4+a wt％Li2CO3-Bi2O3
wherein 0 < a < 4, Li2CO3:Bi2O3The mass ratio of (a) to (b) is 0.25 to 4.
2. A method of making a dielectric ceramic material as claimed in claim 1, comprising the steps of:
(1) according to SrCO3:CeO2The raw material SrCO is weighed according to the molar ratio of 2:13And CeO2Powder is subjected to ball milling and mixing for 4 hours; pre-burning for 4h at 1150 ℃, and performing secondary ball milling to obtain Sr2CeO4A ceramic base material;
(2) according to Sr2CeO4With Li2CO3-Bi2O3A, Li in a mass ratio of (100-a)2CO3-Bi2O3Li in (1)2CO3And Bi2O3Taking raw material Li with the mass ratio of x to y being 0.25-42CO3And Bi2O3Powder; sr is2CeO4Ceramic base material, Li2CO3And Bi2O3Ball milling and mixing the powder, and then drying;
(3) adding the mixed powder prepared in the step (2) into a polyvinyl alcohol solution, and uniformly mixing; pressing under the pressure of 120MPa to prepare a cylindrical blank;
(4) and (4) sintering the blank obtained in the step (3) for 4 hours at the temperature of 875-.
3. The method according to claim 2, wherein in the step (1), the ball milling and mixing are performed under ethanol infiltration conditions.
4. The method according to claim 2, wherein in the step (3), the mass fraction of the polyvinyl alcohol solution is 15%, and the mixed powder material accounts for 8% of the mass of the polyvinyl alcohol solution.
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CN116143514A (en) * 2023-02-22 2023-05-23 苏州博恩希普新材料科技有限公司 Microwave dielectric ceramic and preparation method thereof
CN116535212A (en) * 2023-05-15 2023-08-04 中国矿业大学 High-performance microwave dielectric ceramic material applied to LTCC (Low temperature Co-fired ceramic) and preparation method thereof

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CN113754434A (en) * 2021-08-17 2021-12-07 浙江大学 Strontium cerate-based microwave dielectric ceramic material with medium dielectric constant and preparation method thereof
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CN116143514B (en) * 2023-02-22 2024-03-22 苏州博恩希普新材料科技有限公司 Microwave dielectric ceramic and preparation method thereof
CN116535212A (en) * 2023-05-15 2023-08-04 中国矿业大学 High-performance microwave dielectric ceramic material applied to LTCC (Low temperature Co-fired ceramic) and preparation method thereof
CN116535212B (en) * 2023-05-15 2023-12-26 中国矿业大学 High-performance microwave dielectric ceramic material applied to LTCC (Low temperature Co-fired ceramic) and preparation method thereof

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