CN104844206A - Preparation method of high-performance microwave dielectric ceramic material - Google Patents

Preparation method of high-performance microwave dielectric ceramic material Download PDF

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Publication number
CN104844206A
CN104844206A CN201510196581.5A CN201510196581A CN104844206A CN 104844206 A CN104844206 A CN 104844206A CN 201510196581 A CN201510196581 A CN 201510196581A CN 104844206 A CN104844206 A CN 104844206A
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preparation
ceramic material
microwave
ball
microwave dielectric
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CN104844206B (en
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仇亮
左泽文
金飞
石礼伟
夏往所
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China University of Mining and Technology CUMT
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China University of Mining and Technology CUMT
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Abstract

The invention discloses a preparation method of high-performance microwave dielectric ceramic material. The method comprises the following steps: weighing and burdening the following chemical raw materials: ZnO, ZrO2 and Nb2O5 according to a stoichiometric formula of ZnZrNb2O8, carrying out ball milling, drying, adding 6-10wt% of paraffin, uniformly grinding, sieving, carrying out compaction molding to prepare a green body, and sintering at 1075-1225DEG C to prepare the high-performance microwave dielectric ceramic material. The preparation process is optimized on the basis of a traditional solid phase reaction method, the dielectric constant of the material is 22.13-27.21, the quality factor (Q*f) of the material is 37,000-75,000GHz, and the preparation method has the advantages of reduction of secondary ball milling and calcining technologies, technologic cycle shortening, resource saving, pollution-free process, and wide application prospect.

Description

A kind of preparation method of high performance microwave medium ceramic material
Technical field
The invention relates to a kind of electronic information material and components and parts, particularly a kind of preparation method of high performance microwave medium ceramic material.
Background technology
Along with the development of mobile communication, the miniaturization of microwave device, integrated, high frequency and cost degradation become development trend.Microwave dielectric ceramic materials becomes one of critical material of microwave device development owing to having higher specific inductivity, low-dielectric loss and stable temperature coefficient of resonance frequency.Theoretical and experiment all proves, the various microwave devices made with microwave-medium ceramics, as dielectric resonator, wave filter and microwave-medium antenna etc. are widely used in the every field of microwave technology.
ABNb 2o 8(A=Zn, Mg, Co, Ni, Mn; B=Ti, Zr) type niobate belongs to microwave dielectric ceramic with medium dielectric constant system, and this kind of microwave-medium ceramics, owing to having good microwave dielectric property and relatively low sintering temperature, attracts wide attention.Wherein ZnZrNb 2o 8microwave-medium ceramics was just in the news in recent years, its microwave dielectric property excellence (ε r=30.8, Q × f=62500GHz), be a kind of novel microwave dielectric material very with application prospect.At present, ZnZrNb 2o 8the preparation of microwave dielectric ceramic materials uses traditional solid reaction process usually, and key step is: a ball milling, and oven dry is sieved, calcining, secondary ball milling, and oven dry is sieved, shaping, sintering etc.This preparation method's step is more, and process cycle is long, and particularly secondary ball milling is longer with calcining holding time.
Summary of the invention
Object of the present invention, is to optimize ZnZrNb 2o 8the preparation method of microwave-medium ceramics, provide a kind of relative to conventional process flow, preparation technology is simple, processing step is less, and can obtain the microwave dielectric ceramic materials of higher figure of merit.
The present invention is achieved by following technical solution.
A preparation method for high performance microwave medium ceramic material, has following steps:
(1) by chemical feedstocks ZnO, ZrO 2, Nb 2o 5stoichiometrically formula ZnZrNb 2o 8weigh batching;
(2) chemical feedstocks mixing step (1) configured, to expect: deionized water: the mass ratio of zirconium ball is that 1:1:1.5 adds in ball grinder, and Ball-milling Time is 6 ~ 12 hours;
(3) raw material after step (2) ball milling is placed in loft drier in 100 DEG C of oven dry;
(4) the powder China and foreign countries after step (3) is dried add the paraffin that mass percent is 6 ~ 10%, are placed on resistance furnace and grind even, cross 80 mesh sieves;
(5) the powder powder compressing machine compression moulding after step (4) being sieved is base substrate;
(6) by the base substrate of step (5) in 1075 ~ 1225 DEG C of sintering, be incubated 4 ~ 6 hours, make the microwave-medium ceramics of high quality factor.
The sintering temperature of described step (6) is 1200 DEG C.
The present invention, on the basis of conventional solid reaction method, optimizes ZnZrNb 2o 8the preparation technology of microwave dielectric ceramic materials, and improve ZnZrNb 2o 8the microwave dielectric property of pottery.The present invention compared with the prior art comparatively, decreases secondary ball milling and calcining process, simplify technical process, shorten process cycle, economize on resources, and process is pollution-free, have broad application prospects.Utilize the ZnZrNb that preparation method provided by the invention obtains 2o 8microwave dielectric ceramic materials, its specific inductivity is 22.13 ~ 27.21, and quality factor (Q × f) are 37,000 ~ 75,000GHz; Compared with prior art, its quality factor obtain optimization, improve 10,000GHz.
Embodiment
The present invention adopts chemical feedstocks ZnO (analytical pure), ZrO 2(analytical pure), Nb 2o 5(analytical pure) prepares ZnZrNb 2o 8microwave-medium ceramics.Embodiment is as follows:
(1) by chemical feedstocks ZnO, ZrO 2, Nb 2o 5stoichiometrically formula ZnZrNb 2o 8weigh batching;
(2) the chemical feedstocks mixing will configured, to expect: deionized water: the mass ratio of zirconium ball is that 1:1:1.5 adds in ball grinder, ball milling 6 ~ 12 hours on planetary ball mill;
(3) raw material after ball milling is placed in loft drier in 100 DEG C of oven dry;
(4) the powder China and foreign countries after step (3) is dried add the paraffin that mass percent is 10%, are placed on resistance furnace and grind even, cross 80 mesh sieves;
(5) powder after step (4) being sieved uses powder compressing machine with the green body cylinders of the pressure forming of 8MPa for Φ 10mm × 5mm again;
(6) by base substrate in 1075 ~ 1225 DEG C of sintering, be incubated 4 ~ 6 hours, make the microwave dielectric ceramic materials of high quality factor;
Finally, the microwave dielectric ceramic materials network analyzer of above-mentioned specific embodiment is tested its microwave dielectric property.
Related process parameters and the microwave dielectric property thereof of the specific embodiment of the invention refer to table 1.
Table 1

Claims (2)

1. a preparation method for high performance microwave medium ceramic material, has following steps:
(1) by chemical feedstocks ZnO, ZrO 2, Nb 2o 5stoichiometrically formula ZnZrNb 2o 8weigh batching;
(2) chemical feedstocks mixing step (1) configured, with raw material: deionized water: the mass ratio of zirconium ball is that 1:1:1.5 adds in ball grinder, and Ball-milling Time is 6 ~ 12 hours;
(3) raw material after step (2) ball milling is placed in loft drier in 100 DEG C of oven dry;
(4) the powder China and foreign countries after step (3) is dried add the paraffin that mass percent is 6 ~ 10%, are placed on resistance furnace and grind even, cross 80 mesh sieves;
(5) the powder powder compressing machine compression moulding after step (4) being sieved is base substrate;
(6) by the base substrate of step (5) in 1075 ~ 1225 DEG C of sintering, be incubated 4 ~ 6 hours, make the microwave-medium ceramics of high quality factor.
2. the preparation method of a kind of high performance microwave medium ceramic material according to claim 1, is characterized in that, the sintering temperature of described step (6) is 1200 DEG C.
CN201510196581.5A 2015-04-23 2015-04-23 A kind of preparation method of high performance microwave medium ceramic material Expired - Fee Related CN104844206B (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105174949A (en) * 2015-08-31 2015-12-23 天津大学 Low-loss zinc-zirconium-niobium microwave dielectric ceramic
CN105272245A (en) * 2015-10-30 2016-01-27 天津大学 Low-loss zinc zirconium and niobium series microwave dielectric ceramic prepared by reaction sintering method
CN114656261A (en) * 2022-03-28 2022-06-24 电子科技大学 LTCC microwave dielectric ceramic material with medium dielectric constant and preparation method thereof
CN114804897A (en) * 2022-05-05 2022-07-29 江苏科技大学 Sintering aid for ceramic and preparation method thereof, zinc zirconate microwave dielectric ceramic and preparation method thereof
CN115010490A (en) * 2022-06-29 2022-09-06 安徽大学 Ultralow-loss niobium zinc zirconate microwave dielectric ceramic material and preparation method thereof
CN115124340A (en) * 2022-06-29 2022-09-30 安徽大学 Medium low-loss low-temperature co-fired ceramic material and preparation method and application thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1975939A (en) * 2006-12-04 2007-06-06 天津大学 High-dielectric constant microwave dielectric ceramic and producing method thereof
CN102153343A (en) * 2011-01-10 2011-08-17 天津大学 Method for preparing high Q-value magnesium titanate base microwave medium ceramics by adopting reactive sintering method
CN102603297A (en) * 2012-04-05 2012-07-25 天津大学 Novel low-temperature sintered microwave dielectric ceramic and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1975939A (en) * 2006-12-04 2007-06-06 天津大学 High-dielectric constant microwave dielectric ceramic and producing method thereof
CN102153343A (en) * 2011-01-10 2011-08-17 天津大学 Method for preparing high Q-value magnesium titanate base microwave medium ceramics by adopting reactive sintering method
CN102603297A (en) * 2012-04-05 2012-07-25 天津大学 Novel low-temperature sintered microwave dielectric ceramic and preparation method thereof

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105174949A (en) * 2015-08-31 2015-12-23 天津大学 Low-loss zinc-zirconium-niobium microwave dielectric ceramic
CN105272245A (en) * 2015-10-30 2016-01-27 天津大学 Low-loss zinc zirconium and niobium series microwave dielectric ceramic prepared by reaction sintering method
CN114656261A (en) * 2022-03-28 2022-06-24 电子科技大学 LTCC microwave dielectric ceramic material with medium dielectric constant and preparation method thereof
CN114656261B (en) * 2022-03-28 2023-06-02 电子科技大学 Medium dielectric constant LTCC microwave dielectric ceramic material and preparation method thereof
CN114804897A (en) * 2022-05-05 2022-07-29 江苏科技大学 Sintering aid for ceramic and preparation method thereof, zinc zirconate microwave dielectric ceramic and preparation method thereof
CN114804897B (en) * 2022-05-05 2023-02-28 江苏科技大学 Sintering aid for ceramic and preparation method thereof, zinc zirconate microwave dielectric ceramic and preparation method thereof
CN115010490A (en) * 2022-06-29 2022-09-06 安徽大学 Ultralow-loss niobium zinc zirconate microwave dielectric ceramic material and preparation method thereof
CN115124340A (en) * 2022-06-29 2022-09-30 安徽大学 Medium low-loss low-temperature co-fired ceramic material and preparation method and application thereof
CN115124340B (en) * 2022-06-29 2023-02-28 安徽大学 Medium low-loss low-temperature co-fired ceramic material and preparation method and application thereof

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