CN107162592A - A kind of columbate microeave medium ceramic material and preparation method thereof - Google Patents
A kind of columbate microeave medium ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of columbate microeave medium ceramic material, synthetic expression formula is：ZnZr1‑xMnxNb2O8, wherein x=0.02~0.2.First by ZnO, ZrO2、Nb2O5、MnO2Stoichiometrically formula carries out dispensing；By ball milling, drying, sieving, then at 950 DEG C of calcinings, pressure forming is base substrate after granulation, and required microwave-medium ceramics are made in 1100 DEG C~1200 DEG C sintering in base substrate.Permittivity ε of the present inventionrFor 24.23~29.29, quality factor q × f is 23652~57678GHz, temperature coefficient of resonance frequency τfFor 30.24~4.37 × 10‑6/℃；And preparation technology is simple, intermediate sintering temperature has saved preparation cost, and application prospect is extensive.
Description
Technical field
The invention belongs to a kind of ceramic composition being characterized with composition, more particularly to one kind is with ZnZr1-xMnxNb2O8For
The intermediate sintering temperature of chemical formula, microwave dielectric ceramic materials with medium dielectric constant microwave medium and preparation method thereof.
Background technology
With the fast development of material science, further miniaturization and the requirement of high-quality are still following main rotation to device
Rule, but because current each frequency range is different to the demand of signal quality, therefore realize that device is small for microwave dielectric material in application
For type, emphasis is to ensure that dielectric material has high quality factor.And in addition, optimize the resonant frequency temperature of material
Coefficient, is also the important topic in terms of materials application.
Microwave dielectric material is with the dielectric constant (ε) of its seriation, higher quality factor (Qf), relatively small resonance
Frequency-temperature coefficient (τf) be widely used in making the microwave passive devices such as resonator, wave filter, diectric antenna, medium guided wave
Part, meets the requirement of the development such as mobile communication, satellite communication and military radar.These passive devices are in miniaturization, high-quality
Comparing traditional passive device in terms of change has larger lifting.
ZnZrNb2O8As a kind of novel microwave dielectric ceramic material, because it has moderate dielectric constant, higher Qf
It is worth and receives significant attention.The ZnZrNb of pure phase2O8The microwave dielectric property of material is：Qf=61000GHz, εr=30, τf=-
52×10-6/℃.The shortcoming of its prior art is that quality factor need further raising, and temperature coefficient is unadjustable.
The content of the invention
The purpose of the present invention, is to further improve ZnZrNb2O8The quality factor of medium ceramic material, and certain
Its temperature stability is lifted in degree, to adapt to electronic information technology high frequency and digitized developing direction.With ZnO, ZrO2、
Nb2O5、MnO2For raw material, using simple solid phase method, a kind of ZnZr with high quality factor is prepared1-xMnxNb2O8Microwave-medium
Ceramic material.
The present invention is achieved by following technical solution.
A kind of columbate microeave medium ceramic material, synthetic expression formula is：ZnZr1-xMnxNb2O8, wherein x=0.02~
0.2；
The preparation method of the columbate microeave medium ceramic material, is comprised the following steps that：
(1) by ZnO, ZrO2、Nb2O5、MnO2Stoichiometrically formula ZnZr1-xMnxNb2O8, wherein x=0.02~0.2 is carried out
Dispensing；Powder is put into polyester tank, added after deionized water and zirconium ball, ball milling 4~8 hours；
(2) raw material after step (1) ball milling is put into drying box, in 80~120 DEG C of drying, then crosses 40 mesh sieves；
(3) powder after drying, sieving is put into moderate oven, calcined 5~8 hours in 950 DEG C；
(4) additional 0.9%~1.1% polyvinyl alcohol is made as adhesive in the powder after step (3) calcining
Grain, mixed powder is put into ball grinder, adds zirconia ball and deionized water, and ball milling dries sieving after 9~12 hours,
Base substrate is pressed into 4~8MPa pressure with powder compressing machine again；
(5) base substrate of step (4) is incubated 2~8 hours, be made normal with dielectric in 1100 DEG C~1200 DEG C sintering
Several microwave-medium ceramics.
The step (1) carries out ball milling using planetary ball mill, and drum's speed of rotation is 600 revs/min.
The mass ratio of the powder of the step (1) and deionized water and zirconium ball is the ︰ 1 of 1 ︰ 1.
The blank diameter of the step (4) is 10mm, and thickness is 5mm.
The preferred sintering temperature of the step (5) is 1150 DEG C.
The present invention prepares a kind of new microwave dielectric ceramic materials ZnZr by simple solid-phase synthesis1-xMnxNb2O8
(x=0.02~0.2).Its permittivity εrFor 28.359~25.2946, quality factor q × f is 38906~57678GHz, humorous
Vibration frequency temperature coefficient τfFor -25.14~-7.76 × 10-6/℃.Preparation technology is simple, using intermediate sintering temperature, has saved the time
Cost and energy cost, application prospect are extensive.
Embodiment
The present invention is with ZnO (analysis is pure), Nb2O5(analysis is pure), ZrO2(analysis is pure), MnO2(analysis is pure) is initial feed,
Microwave-medium ceramics are prepared by simple solid-phase synthesis.
Embodiment 1
1. by ZnO, Nb2O5、ZrO2、MnO2Stoichiometrically formula ZnZr1-xMnxNb2O8(x=0.02) dispensing, powder are carried out
Match and be：2.4669gZnO、3.7340g ZrO2、7.9750g Nb2O5、0.0908gMnO2.About 20g powders are put into polyester tank
In, zirconia ball and deionized water, ball milling 6 hours on planetary ball mill are added, rotating speed is 600 revs/min；
2. the powder after ball milling is respectively placed in drying box, 40 mesh sieves are crossed after being dried in 100 DEG C；
3. the powder after drying sieving is put into moderate oven, in 950 DEG C of pre-burnings, 4 hours are incubated；
4. the polyvinyl alcohol that 1.1% is added in the powder after step 3 pre-burning is mixed as adhesive, ball milling is put into
In tank, zirconia ball and deionized water are added, ball milling 12 hours crosses 80 mesh sieves after drying, then with powder compressing machine with 6MPa's
Pressure is pressed into base substrate；
5. green compact are incubated 6 hours, microwave dielectric ceramic with medium dielectric constant is made in 1150 DEG C of sintering.
The microwave property of resulting product is tested by Network Analyzer.
Embodiment 2~3
The preparation method of embodiment 2~3 is substantially identical to embodiment 1, is only that x value is different.The x's of each embodiment
The microwave dielectric property of value and correlation refers to table 1.
Table 1
The invention is not limited in above-described embodiment, the change of many details is possible, but therefore this do not run counter to this
The scope and spirit of invention.
Claims (5)
1. a kind of columbate microeave medium ceramic material, synthetic expression formula is：ZnZr1-xMnxNb2O8, wherein x=0.02~
0.2。
The preparation method of the columbate microeave medium ceramic material, is comprised the following steps that：
(1) by ZnO, ZrO2、Nb2O5、MnO2Stoichiometrically formula ZnZr1-xMnxNb2O8, wherein x=0.02~0.2 carries out dispensing；
Powder is put into polyester tank, added after deionized water and zirconium ball, ball milling 4~8 hours；
(2) raw material after step (1) ball milling is put into drying box, in 80~120 DEG C of drying, then crosses 40 mesh sieves；
(3) powder after drying, sieving is put into moderate oven, calcined 5~8 hours in 950 DEG C；
(4) additional 0.9%~1.1% polyvinyl alcohol is granulated as adhesive in the powder after step (3) calcining, will
Mixed powder is put into ball grinder, adds zirconia ball and deionized water, ball milling dries sieving after 9~12 hours, then uses
Powder compressing machine is pressed into base substrate with 4~8MPa pressure；
(5) base substrate of step (4) is incubated 2~8 hours, be made with medium dielectric constant microwave medium in 1100 DEG C~1200 DEG C sintering
Microwave-medium ceramics.
2. a kind of columbate microeave medium ceramic material according to claim 1, it is characterised in that the step (1) is adopted
Ball milling is carried out with planetary ball mill, drum's speed of rotation is 600 revs/min.
3. a kind of columbate microeave medium ceramic material according to claim 1, it is characterised in that the step (1)
The mass ratio of powder and deionized water and zirconium ball is the ︰ 1 of 1 ︰ 1.
4. a kind of columbate microeave medium ceramic material according to claim 1, it is characterised in that the step (4)
Blank diameter is 10mm, and thickness is 5mm.
5. a kind of columbate microeave medium ceramic material according to claim 1, it is characterised in that the step (5)
It is preferred that sintering temperature be 1150 DEG C.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109336596A (en) * | 2018-09-30 | 2019-02-15 | 天津大学 | Magnesium zirconium germanium niobium series microwave dielectric ceramic and preparation method and application with low-k and ultralow dielectric loss |
| 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 |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104310986A (en) * | 2014-10-09 | 2015-01-28 | 天津大学 | High dielectric constant stable-temperature ceramic capacitor dielectric material |
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2017
- 2017-04-26 CN CN201710282281.8A patent/CN107162592A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104310986A (en) * | 2014-10-09 | 2015-01-28 | 天津大学 | High dielectric constant stable-temperature ceramic capacitor dielectric material |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109336596A (en) * | 2018-09-30 | 2019-02-15 | 天津大学 | Magnesium zirconium germanium niobium series microwave dielectric ceramic and preparation method and application with low-k and ultralow dielectric loss |
| 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 |
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