CN105000877A - High-quality-factor temperature-stabilization type microwave dielectric material and preparation method thereof - Google Patents
High-quality-factor temperature-stabilization type microwave dielectric material and preparation method thereof Download PDFInfo
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- CN105000877A CN105000877A CN201510433663.7A CN201510433663A CN105000877A CN 105000877 A CN105000877 A CN 105000877A CN 201510433663 A CN201510433663 A CN 201510433663A CN 105000877 A CN105000877 A CN 105000877A
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- microwave dielectric
- dielectric material
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- high quality
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Abstract
The invention discloses a high-quality-factor temperature-stabilization type microwave dielectric material. The expression of the target compound of the microwave dielectric material is (1-x) Mg0.97Zn0.035TiO3.005-xCaTiO3, wherein x=0.03-0.09. Through a solid phase method, first, MgO, TiO2, ZnO and CaCO3 are batched according to a stoichiometric equation, pre-sintered at 900 DEG C-1150 DEG C after ball grinding, drying and sieving are performed and sintered at 1200 DEG C-1300 DEG C after granulation and pressing forming are performed, so that the high-quality-factor temperature-stabilization type microwave dielectric ceramic is obtained. The dielectric constant Epsilon r is 18.85-21.98, Q*f is 58.437 GHz-145.467 GHz, and the resonance frequency temperature coefficient Tau f -39.344-33.477* 10<-6> /DEG C. The preparation technology is simplified, and time and the energy cost are saved. The high-quality-factor temperature-stabilization type microwave dielectric material is free of pollution in the process and has broad application prospects.
Description
Technical field
The invention belongs to a kind of take composition as the ceramic composition of feature, particularly relates to a kind of with (1-x) Mg
0.97zn
0.035tiO
3.005– xCaTiO
3what (x=0.03 ~ 0.09) was chemical formula has low-loss, high quality factor, microwave-medium ceramics of the temperature coefficient of resonance frequency of nearly zero and preparation method thereof
Background technology
The development of nearly more than ten years short-wave communication tedhnology, particularly the developing rapidly of mobile communication and satellite communication technology, traditional metal chamber resonator can not meet the demand of application, and the demand of market to the microwave-medium ceramics being applied to the novel microwave such as dielectric resonator, dielectric filter components and parts is day by day vigorous.Microwave device needs at different operate at ambient temperature.Make the carrier signal of wave filter not occur drift at different temperature, just necessarily require the resonant frequency of microwave dielectric material not vary with temperature, or change is less, namely requires the temperature coefficient of resonance frequency of microwave dielectric material nearly zero.Therefore, the temperature stability of microwave dielectric material is the key factor realizing microwave device high stability and high reliability.
Along with the development of stupalith, for meeting different application, the novel material of various excellent performance continues to bring out.Magnesium titanate base system row stupalith is owing to having higher quality factor, and abundant raw material, with low cost, receives and pays close attention to widely.MgTiO
3pottery is as a kind of traditional microwave dielectric material, still there is the microwave dielectric property of its excellence: high quality factor (160,000GHz) in millimere-wave band, suitable specific inductivity (17), but sintering temperature is up to 1450 DEG C, and sintering range is narrow.Therefore, reduce its sintering temperature, improve quality factor, regulating frequency temperature factor is the direction that investigators make great efforts.
Summary of the invention
Object of the present invention is to regulate Mg further
0.97zn
0.035tiO
3.005the temperature coefficient of resonance frequency of microwave-medium ceramics, to adapt to the needs that electronic devices and components use within the scope of differing temps.With MgO, TiO
2, ZnO and CaCO
3for raw material, prepare one by conventional solid-state method and there is high quality factor, (1-x) Mg of near-zero resonance frequency temperature coefficient
0.97zn
0.035tiO
3.005– xCaTiO
3(x=0.03 ~ 0.09) microwave dielectric ceramic materials.
The present invention is achieved by following technical solution.
A kind of high quality factor temperature-stable microwave dielectric material, its target synthetics expression formula is (1-x) Mg
0.97zn
0.035tiO
3.005– xCaTiO
3, wherein x=0.03 ~ 0.09;
The preparation method of this high quality factor temperature-stable microwave dielectric material, concrete implementation step is as follows:
(1) by MgO, TiO
2, ZnO and CaCO
3stoichiometrically formula (1-x) Mg
0.97zn
0.035tiO
3.005– xCaTiO
3, wherein prepare burden in x=0.03 ~ 0.09, first powder put into ball grinder, after adding deionized water and zirconium ball, and ball milling 4 ~ 24 hours;
(2) raw material after step (1) ball milling is put into loft drier, in 100 ~ 120 DEG C of oven dry, then cross 40 mesh sieves;
(3) step (2) is dried, sieve after powder put into moderate oven, in 900 ~ 1150 DEG C of pre-burnings, be incubated 2 ~ 8 hours;
(4) paraffin being 8% ~ 10% using the additional mass percent of powder after step (3) pre-burning carries out granulation as tackiness agent, crosses 80 mesh sieves, makes green compact with powder compressing machine with the pressure of 4 ~ 8MPa;
(5) by the green compact of step (4) in 1200 DEG C ~ 1300 DEG C sintering, be incubated 2 ~ 8 hours, make the temperature-stable microwave-medium ceramics with high quality factor.
(6) microwave dielectric property of network analyzer test microwave dielectric ceramic materials is adopted.
Described step (1) adopts planetary ball mill to carry out ball milling, and drum's speed of rotation is 600 revs/min.
Described step (1) MgO, TiO
2, ZnO and CaCO
3the purity of chemical feedstocks be greater than 99.9%.
The green compact of described step (4), be disk shape, its diameter is 10mm, and thickness is 5mm.
The sintering temperature of described step (5) is 1250 DEG C.
The present invention with MgO, TiO
2, ZnO and CaCO
3for raw material, prepare a kind of novel high quality factor temperature-stabilized microwave medium ceramic material (1-x) Mg by simple solid phase method
0.97zn
0.035tiO
3.005– xCaTiO
3(x=0.03 ~ 0.09).Its DIELECTRIC CONSTANT ε
rbe 18.85 ~ 21.98, Q × f be 58,437 ~ 145,467GHz, temperature coefficient of resonance frequency τ
ffor-39.344 ~ 33.477 × 10
-6/ DEG C.This preparation method saves powder secondary ball milling, simplifies preparation technology, saves time and energy cost.Process is pollution-free, has broad application prospects.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
The present invention is with MgO (analytical pure), TiO
2(analytical pure), ZnO (analytical pure) and CaCO
3(analytical pure) is initial feed, prepares microwave-medium ceramics by simple solid phase method.Step is as follows:
(1) by chemical feedstocks MgO, TiO
2, ZnO and CaCO
3respectively by (1-x) Mg
0.97zn
0.035tiO
3.005– xCaTiO
3(x=0.03 ~ 0.09) stoichiometric ratio is prepared burden.Mixed powder is put into ball grinder, after adding deionized water and zirconium ball, ball milling 12 hours on planetary ball mill, rotating speed is 600 revs/min;
(2) raw material after ball milling is placed in loft drier, in 100 ~ 120 DEG C of oven dry, then crosses 40 mesh sieves;
(3) putting into moderate oven by drying the powder after sieving, in 900 ~ 1150 DEG C of pre-burnings, being incubated 4 hours;
(4) powder after pre-burning is added mass percentage be 8% paraffin wax binder carry out granulation, cross after 80 mesh sieves, powder being pressed into diameter under the pressure of 4MPa with powder compressing machine is 10mm, and thickness is the green compact of about 5mm;
(5) by green compact at 1200 ~ 1300 DEG C of sintering, be incubated 4 hours, make the microwave-medium ceramics with high quality factor;
(6) by the microwave dielectric property of network analyzer test resulting product.
Related process parameters and the microwave dielectric property of specific embodiment refer to table 1.
Table 1
Claims (5)
1. a high quality factor temperature-stable microwave dielectric material, its target synthetics expression formula is (1-x) Mg
0.97zn
0.035tiO
3.005– xCaTiO
3, wherein x=0.03 ~ 0.09;
The preparation method of this high quality factor temperature-stable microwave dielectric material, concrete implementation step is as follows:
(1) by MgO, TiO
2, ZnO and CaCO
3stoichiometrically formula (1-x) Mg
0.97zn
0.035tiO
3.005– xCaTiO
3, wherein prepare burden in x=0.03 ~ 0.09, first powder put into ball grinder, after adding deionized water and zirconium ball, and ball milling 4 ~ 24 hours;
(2) raw material after step (1) ball milling is put into loft drier, in 100 ~ 120 DEG C of oven dry, then cross 40 mesh sieves;
(3) step (2) is dried, sieve after powder put into moderate oven, in 900 ~ 1150 DEG C of pre-burnings, be incubated 2 ~ 8 hours;
(4) paraffin being 8% ~ 10% using the additional mass percent of powder after step (3) pre-burning carries out granulation as tackiness agent, crosses 80 mesh sieves, makes green compact with powder compressing machine with the pressure of 4 ~ 8MPa;
(5) by the green compact of step (4) in 1200 DEG C ~ 1300 DEG C sintering, be incubated 2 ~ 8 hours, make the temperature-stable microwave-medium ceramics with high quality factor.
(6) microwave dielectric property of network analyzer test microwave dielectric ceramic materials is adopted.
2. a kind of high quality factor temperature-stable microwave dielectric material according to claim 1, is characterized in that, described step (1) adopts planetary ball mill to carry out ball milling, and drum's speed of rotation is 600 revs/min.
3. a kind of high quality factor temperature-stable microwave dielectric material according to claim 1, is characterized in that, described step (1) MgO, TiO
2, ZnO and CaCO
3the purity of chemical feedstocks be greater than 99.9%.
4. a kind of high quality factor temperature-stable microwave dielectric material according to claim 1, is characterized in that, the green compact of described step (4), and be disk shape, its diameter is 10mm, and thickness is 5mm.
5. a kind of high quality factor temperature-stable microwave dielectric material according to claim 1, is characterized in that, the sintering temperature of described step (5) is 1250 DEG C.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105601271A (en) * | 2016-01-13 | 2016-05-25 | 南京攀思特电子科技有限公司 | Middle-permittivity microwave dielectric ceramic and manufacturing method thereof |
| CN105801104A (en) * | 2016-02-23 | 2016-07-27 | 天津大学 | High dielectric constant temperature stable type ceramic capacitor dielectric material |
| CN107285761A (en) * | 2017-06-30 | 2017-10-24 | 江苏大学 | A kind of microwave dielectric material and preparation method thereof |
| CN110143814A (en) * | 2019-06-27 | 2019-08-20 | 无锡鑫圣慧龙纳米陶瓷技术有限公司 | A kind of intermediary's temperature-stable microwave-medium ceramics and preparation method thereof |
| CN111377709A (en) * | 2018-12-31 | 2020-07-07 | 深圳市大富科技股份有限公司 | Microwave dielectric ceramic material, dielectric ceramic block and microwave communication equipment |
| CN111377708A (en) * | 2018-12-31 | 2020-07-07 | 深圳市大富科技股份有限公司 | Microwave dielectric ceramic material and preparation method of dielectric ceramic block |
| CN111377732A (en) * | 2018-12-31 | 2020-07-07 | 深圳市大富科技股份有限公司 | Filter, communication equipment, and method for preparing dielectric block and filter |
| CN111548148A (en) * | 2020-06-05 | 2020-08-18 | 陕西华星电子开发有限公司 | Microwave dielectric porcelain, preparation method and application |
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| CN103864414A (en) * | 2014-01-28 | 2014-06-18 | 江苏南瓷绝缘子股份有限公司 | Low-dielectric-constant microwave dielectric ceramic and preparation method thereof |
| CN103992105A (en) * | 2014-04-28 | 2014-08-20 | 天津大学 | High quality factor magnesium titanate based microwave dielectric ceramic and preparation method thereof |
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2015
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| CN103864414A (en) * | 2014-01-28 | 2014-06-18 | 江苏南瓷绝缘子股份有限公司 | Low-dielectric-constant microwave dielectric ceramic and preparation method thereof |
| CN103992105A (en) * | 2014-04-28 | 2014-08-20 | 天津大学 | High quality factor magnesium titanate based microwave dielectric ceramic and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| LINGXIA LI ET AL.: "Influence of CaTiO3 modification on microstructures and microwave dielectric properties of Mg0.97Zn0.03TiO3 ceramics doped with 0.5mol% Zn-excess", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105601271A (en) * | 2016-01-13 | 2016-05-25 | 南京攀思特电子科技有限公司 | Middle-permittivity microwave dielectric ceramic and manufacturing method thereof |
| CN105601271B (en) * | 2016-01-13 | 2018-09-11 | 南京攀思特电子科技有限公司 | A kind of microwave-medium ceramics of medium dielectric constant microwave medium and preparation method thereof |
| CN105801104A (en) * | 2016-02-23 | 2016-07-27 | 天津大学 | High dielectric constant temperature stable type ceramic capacitor dielectric material |
| CN105801104B (en) * | 2016-02-23 | 2018-11-27 | 天津大学 | A kind of high dielectric constant temperature-stable ceramic capacitor dielectric material |
| CN107285761A (en) * | 2017-06-30 | 2017-10-24 | 江苏大学 | A kind of microwave dielectric material and preparation method thereof |
| CN111377709A (en) * | 2018-12-31 | 2020-07-07 | 深圳市大富科技股份有限公司 | Microwave dielectric ceramic material, dielectric ceramic block and microwave communication equipment |
| CN111377708A (en) * | 2018-12-31 | 2020-07-07 | 深圳市大富科技股份有限公司 | Microwave dielectric ceramic material and preparation method of dielectric ceramic block |
| CN111377732A (en) * | 2018-12-31 | 2020-07-07 | 深圳市大富科技股份有限公司 | Filter, communication equipment, and method for preparing dielectric block and filter |
| CN110143814A (en) * | 2019-06-27 | 2019-08-20 | 无锡鑫圣慧龙纳米陶瓷技术有限公司 | A kind of intermediary's temperature-stable microwave-medium ceramics and preparation method thereof |
| CN111548148A (en) * | 2020-06-05 | 2020-08-18 | 陕西华星电子开发有限公司 | Microwave dielectric porcelain, preparation method and application |
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