CN107573069A - A kind of medium dielectric constant microwave medium high q-factor microwave dielectric material of intermediate sintering temperature - Google Patents
A kind of medium dielectric constant microwave medium high q-factor microwave dielectric material of intermediate sintering temperature Download PDFInfo
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Abstract
The invention discloses a kind of medium dielectric constant microwave medium high q-factor microwave dielectric material of intermediate sintering temperature, consisting of (1 x) Zn3Nb2O8‑xAl2O3‑yGeO2, wherein 0<X≤0.09,0<y≤0.30；First by ZnO, Nb2O5By mole 3:Zn is made after 1075 DEG C of pre-burnings in 1 dispensing, ball milling3Nb2O8Solid particle, then by Zn3Nb2O8Solid particle carries out secondary ball milling, and Zn is obtained after drying, sieving3Nb2O8Powder；In Zn3Nb2O8In powder oxide Al is added according to stoichiometric proportion2O3With GeO2, through ball milling, drying, sieving, it is granulated, is pressed into green compact, microwave-medium ceramics is made in 1160~1190 DEG C of sintering in green compact.ε of the present inventionrIt is 90000~100000GHz for 19.5~21, Qf values, temperature coefficient of resonance frequency is 60~70ppm/ DEG C, and sintering temperature is less than 1200 DEG C, and technique is simple, process environmental protection, excellent performance, has and applies future well.
Description
Technical field
The invention belongs to a kind of ceramic composition characterized by composition, more particularly to a kind of Zn3Nb2O8Base dielectric is normal
Number, the microwave dielectric material of high q-factor and preparation method.
Background technology
Higher requirement of the short-wave communication tedhnology fast development in recent years to proposing property of microwave dielectric material system.Microwave
Media ceramic has the characteristics that light weight, cost are low, dielectric constant is high, loss is low, temperature coefficient of resonance frequency is small, is situated between in manufacture
Obtained during the microwave electron component such as matter resonator, dielectric filter, dielectric oscillator, dielectric resonator antenna, duplexer, capacitor
To substantial amounts of application.Intermediary's microwave-medium ceramics refer to microwave-medium ceramics of the dielectric constant 20~50, are commonly used for making
Make various telefilter parts, be used widely in cellular base station, satellite communication.Because dielectric constant range is larger, in
Dielectric microwave medium system species is various.But high-performance, it can meet that the medium system of practical application request is still less.In addition, pass
The intermediary of system, high performance microwave medium system, mostly with higher sintering temperature (>1450 DEG C) so that the collection of microwave device
It is restricted into change.Develop the intermediary of new intermediate sintering temperature, high performance microwave dielectric material is still current study hotspot
With difficult point.
It is provided by the invention that (1-x) Zn is prepared for using conventional solid-state method3Nb2O8-xAl2O3-yGeO2Microwave dielectric material,
The medium system of acquisition has intermediary, a high-Q microwave dielectric properties, and dielectric constant is 19.5~22, and quality factor are 90000~
100000GHz, temperature coefficient of resonance frequency are -60~-70ppm/ DEG C, and the sintering temperature of system is in 1160~1190 DEG C
Temperature sintering, is a kind of very promising intermediary's microwave dielectric material.
The content of the invention
The purpose of the present invention, it is the relatively low quality factor for overcoming existing intermediary's system and too high sintering temperature, it is difficult to full
The shortcomings that sufficient high performance microwave device integrated development demand and deficiency, there is provided a kind of medium dielectric constant microwave medium of intermediate sintering temperature, high q-factor
Microwave dielectric material.
The present invention is achieved by following technical solution.
The medium dielectric constant microwave medium high q-factor microwave dielectric material of a kind of intermediate sintering temperature, consisting of (1-x) Zn3Nb2O8-xAl2O3-
yGeO2, wherein 0<X≤0.09,0<y≤0.30；
The Zn3Nb2O8Raw material composition and molar percentage be ZnO:Nb2O5=3:1.
The preparation method of the medium dielectric constant microwave medium high q-factor microwave dielectric material of above-mentioned intermediate sintering temperature, has following steps：
(1) by ZnO, Nb2O5By mole 3:1 dispensing, with absolute ethyl alcohol mixing and ball milling 8h, dry after 1075 DEG C
Pre-burning 4h, Zn is made3Nb2O8Solid particle；
(2) by Zn obtained by step (1) pre-burning3Nb2O8Solid particle carries out secondary ball milling, Ball-milling Time in absolute ethyl alcohol
8h, 80 mesh sieves are crossed after drying and obtain Zn3Nb2O8Powder；
(3) in Zn obtained by step (2)3Nb2O8In powder, according to (1-x) Zn3Nb2O8-xAl2O3-yGeO2, wherein 0≤x≤
The stoichiometric equation addition oxide Al of 0.09,0≤y≤0.302O3With GeO2, the ball milling 8h in absolute ethyl alcohol, be modified with
The Qf values of lifting system；
(4) by after raw material powder drying obtained by step (3), 80 mesh sieves are crossed, then the concentration that additional mass percent is 0.8%
It is granulated for the 4wt% PVA aqueous solution, then crosses 200 mesh sieves, green compact are pressed under 200MPa pressure；
(5) by green compact obtained by step (4) by the way of lid burns, in 1160~1190 DEG C of sintering, 6h is incubated, medium temperature is made
The microwave-medium ceramics of the medium dielectric constant microwave medium high q-factor of sintering.
The sintering process of the step (5) is：200 DEG C of exclusion crystallizations water first are warming up to through 1~2h, then are heated up through 3~4h
The organic matters such as PVA are excluded to 550 DEG C, then 1160~1190 DEG C are risen to by 110~130min, 6h is incubated, crystal grain is grown up, arrange
Except stomata, the microwave-medium ceramics of the medium dielectric constant microwave medium high q-factor of obtained intermediate sintering temperature.
(1-x) Zn provided by the invention3Nb2O8-xAl2O3-yGeO2Microwave dielectric material, at 1160~1190 DEG C
Sinter porcelain into, it is high into porcelain consistency, compared to the Zn of pure phase3Nb2O8, system dielectric constant do not have significant change, εrFor 19.5~
21, Qf values are 90000~100000GHz (improving 20%), and temperature coefficient of resonance frequency is -60~-70ppm/ DEG C, is situated between in addition
Plastidome sintering temperature is less than 1200 DEG C.Preparation technology of the present invention is simple, process environmental protection, excellent performance, is that one kind has future
Medium dielectric constant microwave medium, the microwave dielectric material of high q-factor.
Embodiment
Below by specific embodiment, the invention will be further described.
A kind of preparation method of the medium dielectric constant microwave medium high q-factor microwave dielectric material of intermediate sintering temperature of the present invention, step are as follows：
(1) present invention is using analysis pure raw material, by ZnO, Nb2O5By matter molar percentage 3:1 dispensing, is mixed with absolute ethyl alcohol
Dried after closing ball milling 8h and in 1075 DEG C of pre-burning 4h, Zn is made3Nb2O8Solid particle；
(2) by Zn obtained by step (1) pre-burning3Nb2O8Solid particle carries out secondary ball milling, Ball-milling Time in absolute ethyl alcohol
8h, after drying, cross 80 mesh sieves and obtain Zn3Nb2O8Powder；
(3) in Zn obtained by step (2)3Nb2O8In powder, according to (1-x) Zn3Nb2O8-xAl2O3-yGeO2, wherein 0<x≤
0.09,0<The stoichiometric equation addition oxide Al of y≤0.302O3With GeO2, the ball milling 8h in absolute ethyl alcohol, be modified with
The Qf values of lifting system；
(4) by after raw material powder drying obtained by step (3), 80 mesh sieves are crossed, then the concentration that additional mass percent is 0.8%
It is granulated for the 4wt% PVA aqueous solution, then crosses 200 mesh sieves, green compact are pressed under 200MPa pressure；
(5) mode burnt using lid is sintered, and by the green compact of different doping contents, batch sintering, 200 is warming up to through 1~2h
DEG C the crystallization water is excluded, be warming up to 550 DEG C of exclusion organic matters such as PVA through 3~4h, 1160~1190 are risen to by 110~130min
DEG C, 6h is incubated, crystal grain is grown up, excludes stomata, so as to which the medium dielectric constant microwave medium high q-factor microwave-medium of fine and close intermediate sintering temperature be made
Ceramics.
Finally by Network Analyzer and the microwave dielectric property of dependence test fixture test article.
The important technological parameters and its dielectric properties test result of the specific embodiment of the invention 1~22 refer to table 1.
τ in table 1fTest temperature section be 25~85 DEG C.
Table 1
(1-x) Zn provided by the invention3Nb2O8-xAl2O3-yGeO2The microwave dielectric material of medium dielectric constant microwave medium, high q-factor, burn
1160~1190 DEG C of junction temperature, high into porcelain consistency, the medium system finally obtained has excellent microwave dielectric property, such as
Under：
Dielectric constant：19.5~22.1；
Quality factor：90000~100000GHz；
Temperature coefficient of resonance frequency：- 60~-70ppm/ DEG C.
Claims (2)
- A kind of 1. medium dielectric constant microwave medium high q-factor microwave dielectric material of intermediate sintering temperature, consisting of (1-x) Zn3Nb2O8-xAl2O3- yGeO2, wherein 0<X≤0.09,0<y≤0.30；The Zn3Nb2O8Raw material composition and molar percentage be ZnO:Nb2O5=3:1.The preparation method of the medium dielectric constant microwave medium high q-factor microwave dielectric material of above-mentioned intermediate sintering temperature, has following steps：(1) by ZnO, Nb2O5By mole 3:1 dispensing, with absolute ethyl alcohol mixing and ball milling 8h, dry after 1075 DEG C of pre-burnings 4h, Zn is made3Nb2O8Solid particle；(2) by Zn obtained by step (1) pre-burning3Nb2O8Solid particle carries out secondary ball milling in absolute ethyl alcohol, Ball-milling Time 8h, dries 80 mesh sieves are crossed after dry and obtain Zn3Nb2O8Powder；(3) in Zn obtained by step (2)3Nb2O8In powder, according to (1-x) Zn3Nb2O8-xAl2O3-yGeO2, wherein 0≤x≤ The stoichiometric equation addition oxide Al of 0.09,0≤y≤0.302O3With GeO2, the ball milling 8h in absolute ethyl alcohol, be modified with The Qf values of lifting system；(4) by after raw material powder drying obtained by step (3), 80 mesh sieves are crossed, then the concentration that additional mass percent is 0.8% is The 4wt% PVA aqueous solution is granulated, and then crosses 200 mesh sieves, green compact are pressed under 200MPa pressure；(5) by green compact obtained by step (4) by the way of lid burns, in 1160~1190 DEG C of sintering, 6h is incubated, intermediate sintering temperature is made Medium dielectric constant microwave medium high q-factor microwave-medium ceramics.
- 2. a kind of medium dielectric constant microwave medium high q-factor microwave dielectric material of intermediate sintering temperature according to claim 1, its feature exist In the sintering process of the step (5) is：200 DEG C of exclusion crystallizations water first are warming up to through 1~2h, then 550 are warming up to through 3~4h DEG C the organic matter such as PVA is excluded, then 1160~1190 DEG C are risen to by 110~130min, be incubated 6h, crystal grain is grown up, exclude gas Hole, the microwave-medium ceramics of the medium dielectric constant microwave medium high q-factor of intermediate sintering temperature are made.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109912306A (en) * | 2019-03-06 | 2019-06-21 | 天津大学 | A kind of adjustable high q-factor microwave-medium ceramics of temperature coefficient of resonance frequency |
| CN113213912A (en) * | 2020-02-05 | 2021-08-06 | 天津大学 | High-performance novel medium scheelite structure medium material and preparation method thereof |
Citations (5)
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| JPS56155070A (en) * | 1980-04-26 | 1981-12-01 | Kyoritsu Ceramic Materials | Raw material composition for manufacturing high dielectric constant ceramic |
| TW200427652A (en) * | 2003-06-11 | 2004-12-16 | Walsin Technology Corp | Low temperature co-fired ceramic material with high microwave characteristics and its manufacturing method |
| 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 |
| CN103964847A (en) * | 2014-04-23 | 2014-08-06 | 天津大学 | Low-loss micorwave dieleertic ceramic material for chip type multi-layer ceramic capacitor |
| CN106986635A (en) * | 2017-03-31 | 2017-07-28 | 天津大学 | A kind of intermediate sintering temperature ceramics as low-loss microwave medium material and preparation method thereof |
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2017
- 2017-09-27 CN CN201710889788.XA patent/CN107573069A/en active Pending
Patent Citations (5)
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|---|---|---|---|---|
| JPS56155070A (en) * | 1980-04-26 | 1981-12-01 | Kyoritsu Ceramic Materials | Raw material composition for manufacturing high dielectric constant ceramic |
| TW200427652A (en) * | 2003-06-11 | 2004-12-16 | Walsin Technology Corp | Low temperature co-fired ceramic material with high microwave characteristics and its manufacturing method |
| 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 |
| CN103964847A (en) * | 2014-04-23 | 2014-08-06 | 天津大学 | Low-loss micorwave dieleertic ceramic material for chip type multi-layer ceramic capacitor |
| CN106986635A (en) * | 2017-03-31 | 2017-07-28 | 天津大学 | A kind of intermediate sintering temperature ceramics as low-loss microwave medium material and preparation method thereof |
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| PENPHITCHA AMONPATTARATKIT ET AL.: ""Microstructure and dielectric properties of Zn3Nb2O8 ceramics prepared by a two-stage sintering method"", 《CERAMICS INTERNATIONAL》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109912306A (en) * | 2019-03-06 | 2019-06-21 | 天津大学 | A kind of adjustable high q-factor microwave-medium ceramics of temperature coefficient of resonance frequency |
| CN113213912A (en) * | 2020-02-05 | 2021-08-06 | 天津大学 | High-performance novel medium scheelite structure medium material and preparation method thereof |
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