CN101747037A - High-Q multiphase microwave dielectric ceramics and preparation method thereof - Google Patents

High-Q multiphase microwave dielectric ceramics and preparation method thereof Download PDF

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CN101747037A
CN101747037A CN200810232456A CN200810232456A CN101747037A CN 101747037 A CN101747037 A CN 101747037A CN 200810232456 A CN200810232456 A CN 200810232456A CN 200810232456 A CN200810232456 A CN 200810232456A CN 101747037 A CN101747037 A CN 101747037A
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microwave dielectric
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刘家骥
高峰
洪荣子
胡国辛
王通
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Northwestern Polytechnical University
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Northwestern Polytechnical University
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Abstract

The invention provides high-Q multiphase microwave dielectric ceramics and a preparation method thereof. A general expression of the ceramics is (1-x)ZnNb2O6 + xZn3Nb2O8, wherein x is more than or equal to 0.1, and less than or equal to 0.4. The preparation method comprises: prefiring ZnO and Nb2O5 into ZnNb2O6; prefiring ZnO and Nb2O5 into Zn3Nb2O8; adding PVA accounting for 3 to 8 weight percent to synthetic ZnNb2O6 and Zn3Nb2O8; performing granulation and compression molding; sintering green bodies; and obtaining the high-Q multiphase microwave dielectric ceramics. The ceramics have high Q*f value and low sintering temperature in a microwave frequency band, and has a dielectric constant of 22 to 24. By utilizing the high-Q multiphase microwave dielectric ceramics provided by the invention, dielectric resonators, filters and other microwave components can be applicable to higher frequency and higher power. Meanwhile, due to the low sintering temperature, cheaper electrode materials can be used so as to save a large amount of energy and reduce application cost.

Description

A kind of high-Q multiphase microwave dielectric ceramics and preparation method thereof
One, technical field
The present invention relates to the microwave dielectric ceramic materials field, specifically is a kind of high-Q multiphase microwave dielectric ceramics and preparation method thereof.
Two, background technology
In recent years, along with developing rapidly of mobile communication and satellite communication technology, the needs of the microwave-medium ceramics that microwave devices such as dielectric resonator and wave filter are used are just growing.Investigate demonstration global mobile phone sales volume in 2007 and reach 11.2 hundred million ones, estimate by two microwave devices of every mobile phone, only mobile phone production just need to 22.4 hundred million microwave devices in 2007.
In addition, the progress of portable mobile communication equipment has caused various owing to multicore sheet high-frequency element or the various types of wiring boards of low temperature high fever pottery (LTCC) generation and the development of multi-chip module, and this just requires device miniaturization, chip type, lightweight.Impel microwave-medium ceramics to realize that lamination burns altogether with other dielectric materials or inductive material, wherein require to have the metal or alloy of good electrical conductivity as interior electrode.And representational so far microwave-medium ceramics compound as: though zirconia titanate tin system, barium oxide-TiO 2 series and have high Q value as tantalum zincic acid barium, BMT, the niobium zincic acid barium of barium-perovskite series, sintering temperature is all at 1300 ℃～1500 ℃.Because its sintering temperature is too high, when the preparation microwave device, can only use to contain the high silver palladium alloy of palladium amount, even pure palladium is as electrode materials.And the market price of palladium is higher than silver far away, has so greatly improved the cost of material of components and parts, and high sintering temperature needs to consume the more energy, the increase preparation cost in preparation process.
At present the technology of reduction sintering temperature commonly used has: chemical synthesis, as sol-gel method etc.; The special sintering method is such as hot pressed sintering, microwave sintering, HIP sintering etc.; Doped sintered auxiliary agent; Select the sintering temperature and low material system for use.But chemical synthesis and special sintering method often need special equipment, and expensive raw material, and complex process, are unfavorable for realizing the suitability for industrialized production needs.In conjunction with selecting sintering temperature and low material system and doped sintered auxiliary agent for use will be a kind of effective ways that reduce sintering temperature.Though and microwave-medium ceramics compound sintering temperatures such as zinc niobate, tantalic acid zinc are at 1100 ℃～1300 ℃, its Q value reduces greatly.So the microwave-medium ceramics that has simultaneously sintering temperature and low and high Q value becomes present technological difficulties.
Three, summary of the invention
In order to overcome expensive raw material price, preparation cost height, energy consumption height and the low problem of material microwave dielectric properties that exists in the prior art.The present invention proposes a kind of high-Q multiphase microwave dielectric ceramics and preparation method thereof.
General expression of the present invention is (1-x) ZnNb 2O 6+ xZn 3Nb 2O 8, 0.1≤x≤0.4 wherein.
Concrete preparation process is as follows:
(1) with purity is 99.9% ZnO and Nb 2O 5, ZnNb is dried, grinds, is pre-fired into to 1: 1 in molar ratio mixing and ball milling then 2O 6, calcined temperature is 1000 ℃～1050 ℃, the pre-burning time is 3～6 hours.
(2) with purity be 99.9% ZnO and Nb 2O 5, Zn is dried, grinds, is pre-fired into to 3: 1 in molar ratio mixing and ball milling then 3Nb 2O 8, calcined temperature is 1100 ℃～1150 ℃, the pre-burning time is 3～6 hours.
(3) with ZnNb 2O 6And Zn 3Nb 2O 89～6: 1～4 mixing and ball milling is dried then in molar ratio, adds PVA (polyvinyl alcohol) granulation of 3wt%～8wt%, produces 200 microns particle, and compression moulding under 100Mpa pressure.
(4) the sample binder removal after the moulding, dump temperature is 500 ℃, and temperature rise rate is 2 ℃/minute, removes binding agent.
(5) with base substrate at 1100 ℃～1150 ℃ sintering, soaking time is 2～6 hours, and under microwave frequency band Q * f value greater than 130000GHz.
The invention provides and have high Q under microwave frequency band * f value (greater than 130000GHz) and sintering temperature and low (1100 ℃), specific inductivity is 22～24 multi-phase microwave dielectric ceramic simultaneously.And utilize high-Q multiphase microwave dielectric ceramics provided by the invention, can make the microwave devices such as dielectric resonator and wave filter be fit to higher frequency and more powerful application.Because sintering temperature and low can use the cheaper electrode material of price, and save a large amount of energy, reduce application cost simultaneously.
Four, description of drawings
Accompanying drawing 1 is ZnNb 2O 6-Zn 3Nb 2O 8The XRD collection of illustrative plates of complex phase ceramic.
Accompanying drawing 2 is schemas of high-Q multiphase microwave dielectric ceramics preparation method.Wherein:
1.Zn 3Nb 2O 82. be ZnNb 2O 6The component of a is 0.9ZnNb 2O 6+ 0.1Zn 3Nb 2O 8
The component of b is 0.8ZnNb 2O 6+ 0.2Zn 3Nb 2O 8The component of c is 0.7ZnNb 2O 6+ 0.3Zn 3Nb 2O 8
The component of d is 0.6ZnNb 2O 6+ 0.4Zn 3Nb 2O 8
Five, embodiment
Further set forth substantive features of the present invention and marked improvement below by embodiment, yet the present invention only limits to described embodiment absolutely not.
Embodiment one:
Present embodiment is take ZnO and the Nb of purity as 99.9% 2O 5Be initiation material, by (1-x) ZnNb 2O 6+ xZn 3Nb 2O 8The stoichiometric proportion batching of (wherein x=0.1).
Preparation process is:
(1) with ZnO and Nb 2O 51: 1 in molar ratio proportioning, with planetary mills mixing and ball milling 12 hours in the polyethylene ball grinder, take absolute ethyl alcohol and zirconium ball as medium, the wet feed behind the ball milling 50 ℃ of oven dry 12 hours, again with agate mortar that dry powder is levigate, place corundum crucible to be pre-fired into ZnNb 2O 6, calcined temperature is 1000 ℃, the pre-burning time is 3 hours.
(2) with ZnO and Nb 2O 53: 1 in molar ratio proportionings, with planetary mills mixing and ball milling 12 hours in the polyethylene ball grinder, take absolute ethyl alcohol and zirconium ball as medium, the wet feed behind the ball milling 50 ℃ of oven dry 12 hours, again with agate mortar that dry powder is levigate, place corundum crucible to be pre-fired into Zn 3Nb 2O 8, calcined temperature is 1100 ℃, the pre-burning time is 3 hours.
(3) with synthetic ZnNb 2O 6And Zn 3Nb 2O 8Mixed in 9: 1 in molar ratio, with planetary mills mixing and ball milling 12 hours in the polyethylene ball grinder, take absolute ethyl alcohol and zirconium ball as medium, the wet feed behind the ball milling was 50 ℃ of oven dry 12 hours.
(4) in the powder of oven dry, add the 3.00wt% polyvinyl alcohol adhesive aqueous solution, ground 2 hours, produce about 200 micron particle, under 100Mpa pressure, be pressed into diameter 12mm, the cylinder sample of thickness 6mm with this particle with agate mortar.
(5) with the sample after the moulding in electric furnace through 500 ℃ of thermal treatments, temperature rise rate is 2 ℃/min, burns binding agent.
(6) will remove the biscuit body of binding agent, 1100 ℃ of sintering 2 hours, temperature rise rate was 5 ℃/min.
Analyze with the ceramic sample of powder x-ray diffraction peak after to sintering, analysis result has formed by ZnNb shown in figure one 2O 6Phase and Zn 3Nb 2O 8The multiphase structure of phase composition.Sample has good microwave dielectric property: ε r=23.01, Q * f=134852GHz (f=8.343GHz).
Embodiment two:
Present embodiment is take ZnO and the Nb of purity as 99.9% 2O 5Be initiation material, by (1-x) ZnNb 2O 6+ xZn 3Nb 2O 8The stoichiometric proportion batching of (wherein x=0.2).
Preparation process is:
(1) with ZnO and Nb 2O 51: 1 in molar ratio proportioning, with planetary mills mixing and ball milling 12 hours in the polyethylene ball grinder, take absolute ethyl alcohol and zirconium ball as medium, the wet feed behind the ball milling 50 ℃ of oven dry 12 hours, again with agate mortar that dry powder is levigate, place corundum crucible to be pre-fired into ZnNb 2O 6, calcined temperature is 1020 ℃, the pre-burning time is 4 hours.
(2) with ZnO and Nb 2O 53: 1 in molar ratio proportionings, with planetary mills mixing and ball milling 12 hours in the polyethylene ball grinder, take absolute ethyl alcohol and zirconium ball as medium, the wet feed behind the ball milling 50 ℃ of oven dry 12 hours, again with agate mortar that dry powder is levigate, place corundum crucible to be pre-fired into Zn 3Nb 2O 8, calcined temperature is 1120 ℃, the pre-burning time is 4 hours.
(3) with synthetic ZnNb 2O 6And Zn 3Nb 2O 8Mixed in 8: 2 in molar ratio, with planetary mills mixing and ball milling 14 hours in the polyethylene ball grinder, take absolute ethyl alcohol and zirconium ball as medium, the wet feed behind the ball milling was 50 ℃ of oven dry 12 hours..
(4) in the powder of oven dry, add the 5.00wt% polyvinyl alcohol adhesive aqueous solution, ground 2 hours, produce about 200 micron particle, under 100Mpa pressure, be pressed into diameter 12mm, the cylinder sample of thickness 6mm with this particle with agate mortar.
(5) with the sample after the moulding in electric furnace through 500 ℃ of thermal treatments, temperature rise rate is 2 ℃/min, burns binding agent.
(6) will remove the biscuit body of binding agent, 1130 ℃ of sintering 3 hours, temperature rise rate was 5 ℃/min.
Analyze with the ceramic sample of powder x-ray diffraction peak after to sintering, analysis result has formed by ZnNb shown in figure one 2O 6Phase and Zn 3Nb 2O 8The multiphase structure of phase composition.Sample has excellent microwave dielectric properties: ε r=22.67, Q * f=130903GHz (f=8.247GHz).
Embodiment three:
Present embodiment is take ZnO and the Nb of purity as 99.9% 2O 5Be initiation material, by (1-x) ZnNb 2O 6+ xZn 3Nb 2O 8The stoichiometric proportion batching of (wherein x=0.3).
Preparation process is:
(1) with ZnO and Nb 2O 51: 1 in molar ratio proportioning, with planetary mills mixing and ball milling 12 hours in the polyethylene ball grinder, take absolute ethyl alcohol and zirconium ball as medium, the wet feed behind the ball milling 50 ℃ of oven dry 12 hours, again with agate mortar that dry powder is levigate, place corundum crucible to be pre-fired into ZnNb 2O 6, calcined temperature is 1040 ℃, the pre-burning time is 5 hours.
(2) with ZnO and Nb 2O 53: 1 in molar ratio proportionings, with planetary mills mixing and ball milling 12 hours in the polyethylene ball grinder, take absolute ethyl alcohol and zirconium ball as medium, the wet feed behind the ball milling 50 ℃ of oven dry 12 hours, again with agate mortar that dry powder is levigate, place corundum crucible to be pre-fired into Zn 3Nb 2O 8, calcined temperature is 1130 ℃, the pre-burning time is 5 hours.
(3) with synthetic ZnNb 2O 6And Zn 3Nb 2O 8Mixed in 7: 3 in molar ratio, with planetary mills mixing and ball milling 14 hours in the polyethylene ball grinder, take absolute ethyl alcohol and zirconium ball as medium, the wet feed behind the ball milling was 50 ℃ of oven dry 12 hours.
(4) in the powder of oven dry, add the 7.00wt% polyvinyl alcohol adhesive aqueous solution, ground 2 hours, produce about 200 micron particle, under 100Mpa pressure, be pressed into diameter 12mm, the cylinder sample of thickness 6mm with this particle with agate mortar.
(5) with the sample after the moulding in electric furnace through 500 ℃ of thermal treatments, temperature rise rate is 2 ℃/min, burns binding agent.
(6) will remove the biscuit body of binding agent, 1120 ℃ of sintering 4 hours, temperature rise rate was 5 ℃/min.
Analyze with the ceramic sample of powder x-ray diffraction peak after to sintering, analysis result has formed by ZnNb shown in figure one 2O 6Phase and Zn 3Nb 2O 8The multiphase structure of phase composition.Sample has excellent microwave dielectric properties: ε r=22.19, Qxf=149642GHz (f=8.115GHz).
Embodiment four:
Present embodiment is take ZnO and the Nb of purity as 99.9% 2O 5Be initiation material, by (1-x) ZnNb 2O 6+ xZn 3Nb 2O 8The stoichiometric proportion batching of (wherein x=0.4).
Preparation process is:
(1) with ZnO and Nb 2O 51: 1 in molar ratio proportioning, with planetary mills mixing and ball milling 12 hours in the polyethylene ball grinder, take absolute ethyl alcohol and zirconium ball as medium, the wet feed behind the ball milling 50 ℃ of oven dry 12 hours, again with agate mortar that dry powder is levigate, place corundum crucible to be pre-fired into ZnNb 2O 6, calcined temperature is 1050 ℃, the pre-burning time is 6 hours.
(2) with ZnO and Nb 2O 53: 1 in molar ratio proportionings, with planetary mills mixing and ball milling 12 hours in the polyethylene ball grinder, take absolute ethyl alcohol and zirconium ball as medium, the wet feed behind the ball milling 50 ℃ of oven dry 12 hours, again with agate mortar that dry powder is levigate, place corundum crucible to be pre-fired into Zn 3Nb 2O 8, calcined temperature is 1150 ℃, the pre-burning time is 6 hours.
(3) with synthetic ZnNb 2O 6And Zn 3Nb 2O 8Mixed in 6: 4 in molar ratio, with planetary mills mixing and ball milling 12 hours in the polyethylene ball grinder, take absolute ethyl alcohol and zirconium ball as medium, the wet feed behind the ball milling was 50 ℃ of oven dry 12 hours.
(4) in the powder of oven dry, add the 8.00wt% polyvinyl alcohol adhesive aqueous solution, ground 2 hours, produce about 200 micron particle, under 100Mpa pressure, be pressed into diameter 12mm, the cylinder sample of thickness 6mm with this particle with agate mortar.
(5) with the sample after the moulding in electric furnace through 500 ℃ of thermal treatments, temperature rise rate is 2 ℃/min, burns binding agent.
(6) will remove the biscuit body of binding agent, 1150 ℃ of sintering 6 hours, temperature rise rate was 5 ℃/min.
Analyze with the ceramic sample of powder x-ray diffraction peak after to sintering, analysis result has formed by ZnNb shown in figure one 2O 6Phase and Zn 3Nb 2O 8The multiphase structure of phase composition.Sample has excellent microwave dielectric properties: ε r=22.16, Q * f=132097GHz (f=8.673GHz).
It is as shown in the table for the microwave dielectric property of sample and sintering temperature among above-mentioned four embodiment:
ZnNb 2O 6Content, 1-x (mol%) Zn 3Nb 2O 8Content, x (mol%) ε r Q * f (GHz) F (GHz) Sintering temperature (℃)
90 10 23.01 134852 8.343 1100
80 20 22.67 130903 8.247 1130
70 30 22.19 149642 8.115 1120
60 40 22.16 132097 8.673 1150

Claims (2)

1. a high-Q multiphase microwave dielectric ceramics is characterized in that, the general expression of this high-Q multiphase microwave dielectric ceramics is (1-x) ZnNb 2O 6+ xZn 3Nb 2O 8, 0.05＜x＜0.50 wherein.
2. one kind prepares the method for high-Q multiphase microwave dielectric ceramics according to claim 1, it is characterized in that, concrete preparation process is:
A. be 99.9% ZnO and Nb with purity 2O 5ZnNb is ground and be pre-fired into to 1: 1 in molar ratio mixing and ball milling, at drying 2O 6Calcined temperature is 950 ℃～1050 ℃, and the pre-burning time is 2～6 hours;
B. be 99.9% ZnO and Nb with purity 2O 5Zn is ground and be pre-fired into to 3: 1 in molar ratio mixing and ball milling, at drying 3Nb 2O 8, calcined temperature is 1050 ℃～1150 ℃, the pre-burning time is 2～6 hours;
C. with ZnNb 2O 6And Zn 3Nb 2O 8Respectively by ceramic composition and ratio mixing and ball milling and oven dry; Add the PVA granulation of 2wt%～10wt%, produce 200 microns particle, and compression moulding under 100Mpa pressure;
D. with the sample binder removal after the moulding; Dump temperature is 500 ℃, and temperature rise rate is 2 ℃/minute; Remove binding agent, obtain base substrate;
E. with base substrate at 1050 ℃～1150 ℃ sintering, soaking time is 2～6 hours, and under microwave frequency band Q * f value greater than 130000GHz.
CN200810232456A 2008-11-28 2008-11-28 High-Q multiphase microwave dielectric ceramics and preparation method thereof Pending CN101747037A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102060532A (en) * 2010-11-12 2011-05-18 西安广芯电子科技有限公司 High-quality factor microwave medium ceramic and preparation method thereof
CN102531601A (en) * 2012-03-05 2012-07-04 昆明理工大学 Liquid phase preparation method for zinc niobate microwave dielectric ceramic
CN102584232A (en) * 2012-01-11 2012-07-18 西北工业大学 Microwave dielectric ceramic and preparation method thereof
CN112142465A (en) * 2020-09-25 2020-12-29 西华大学 Rare earth ion modified filter ceramic for 5G base station and preparation method thereof

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102060532A (en) * 2010-11-12 2011-05-18 西安广芯电子科技有限公司 High-quality factor microwave medium ceramic and preparation method thereof
CN102060532B (en) * 2010-11-12 2013-03-06 西安广芯电子科技有限公司 High-quality factor microwave medium ceramic and preparation method thereof
CN102584232A (en) * 2012-01-11 2012-07-18 西北工业大学 Microwave dielectric ceramic and preparation method thereof
CN102531601A (en) * 2012-03-05 2012-07-04 昆明理工大学 Liquid phase preparation method for zinc niobate microwave dielectric ceramic
CN112142465A (en) * 2020-09-25 2020-12-29 西华大学 Rare earth ion modified filter ceramic for 5G base station and preparation method thereof

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Application publication date: 20100623