CN107056295A - A kind of high-performance zinc zirconium niobium series microwave dielectric ceramic - Google Patents

A kind of high-performance zinc zirconium niobium series microwave dielectric ceramic Download PDF

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CN107056295A
CN107056295A CN201610974137.6A CN201610974137A CN107056295A CN 107056295 A CN107056295 A CN 107056295A CN 201610974137 A CN201610974137 A CN 201610974137A CN 107056295 A CN107056295 A CN 107056295A
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powder
dielectric ceramic
zirconium niobium
zinc zirconium
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肖谧
周子淇
顾青青
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Tianjin University
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    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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Abstract

The invention discloses a kind of high-performance zinc zirconium niobium series microwave dielectric ceramic, consisting of Zn1‑xNixZrNb2O8, wherein 0 ＜ x≤0.08.First by ZnO, ZrO2, Nb2O5And Ni2O3According to Zn1‑ xNixZrNb2O8(0 ＜ x≤0.08) carries out dispensing, by abrading-ball, drying, sieving, in 1000~1100 DEG C of pre-burnings；Additional 8% adhesive is granulated after secondary ball milling, drying again, and compressing is base substrate, and high quality factor zinc zirconium niobium system media ceramic is made in 1,200 1250 DEG C of sintering in base substrate.It is 28.76, the less microwave ceramics medium of temperature coefficient of resonance frequency that the present invention, which successfully obtains Q × f values 73224Ghz, dielectric constant, and preparation technology of the present invention is simple, and process is pollution-free.

Description

A kind of high-performance zinc zirconium niobium series microwave dielectric ceramic
Technical field
The invention belongs to a kind of ceramic composition being characterized with composition, more particularly to a kind of zinc of new high quality factor Zirconium niobium series microwave dielectric ceramic and preparation method thereof.
Background technology
Present mobile communication is developed rapidly, promote all kinds of microwave mobile communication terminal devices to miniaturization, lightweight, The direction of multifunction and cost degradation is fast-developing.Medium for making the basis such as dielectric resonator and critical material is made pottery Porcelain, must meet following characteristics：Higher relative dielectric constant (εr), compared with low-dielectric loss (dielectric loss tangent angle tan δ), become It is bordering on zero temperature coefficient of resonance frequency (τf)。
Zinc zirconium niobium series microwave dielectric ceramic is a kind of new microwave dielectric material with superior microwave dielectric property, its Dielectric constant is about 25, and temperature coefficient of resonance frequency is -52ppm/ DEG C, and sintering temperature is 1250 DEG C.But its Q × f value is relatively low, is 61000 or so.The present invention uses conventional solid-state method, prepares the Zn of higher figure of merit1-xNixZrNb2O8Microwave-medium ceramics, Improve temperature coefficient of resonance frequency simultaneously, preferably can be applied among microwave regime.
The content of the invention
The purpose of the present invention, is to overcome prior art Q × relatively low shortcoming of f values (61000 or so), with ZnO, ZrO2, Nb2O5, Ni2O3For primary raw material, there is provided a kind of zinc zirconium niobium system microwave ceramics with higher figure of merit, excellent dielectric performance Medium.
The high-performance zinc zirconium niobium series microwave dielectric ceramic of the present invention, consisting of Zn1-xNixZrNb2O8, wherein 0 ＜ x≤ 0.08；
The preparation method of above-mentioned high-performance zinc zirconium niobium series microwave dielectric ceramic, has steps of：
(1) by raw material ZnO, ZrO2、Nb2O5And Ni2O3, by chemical formula Zn1-xNixZrNb2O8, wherein x=0~0.08 is carried out Dispensing, then powder is put into ball grinder, add deionized water and zirconia ball, ball milling 6~8 hours on ball mill；
(2) powder after step (1) ball milling is placed under 110 DEG C of oven conditions and dried, after after raw material drying, sieving is obtained Obtain evengranular powder；
(3) powder for being well mixed step (2) carries out pre-burning in 1000~1100 DEG C, and burn-in time is 1~4 hour；
(4) ceramic powder after step (3) pre-burning is put into ball grinder, deionized water and zirconia ball is added, in ball Secondary ball milling 6~8 hours on grinding machine；Additional 8% adhesive is granulated in ceramic powder after air-drying, and crosses 80 mesh sieves, then use Powder compressing machine is shaped to base substrate；
(5) base substrate of step (4) is incubated 1~8 hour in 1200-1250 DEG C of sintering, the zinc zirconium of high quality factor is made Niobium system
Raw material ZnO, ZrO of the step (1)2、Nb2O5And Ni2O3Quality purity be more than 99.9%.
Step (3) calcined temperature is 1075 DEG C.
The step (1), the raw material of step (4) ball-milling technology, the mass ratio of deionized water and zirconia ball are 2:16: 15。
The pressure of the powder compressing machine of the step (4) is 2~8Mpa.
The blank diameter of the step (4) is 10~20mm, and thickness is 2~8mm.
The sintering temperature of the step (5) is 1250 DEG C.
The present invention is based on zinc zirconium niobium microwave-medium ceramics, the Ni for certain content of adulterating2O3, successfully obtain quality Factor height (Q × f value 73224Ghz), dielectric constant 28.76, the less microwave-medium ceramics of temperature coefficient of resonance frequency.This hair Bright preparation technology is simple, and process is pollution-free, improves its quality factor, is a kind of up-and-coming microwave dielectric material.
Embodiment
The present invention is more than 99.9% chemical raw material ZnO, ZrO using purity2、Nb2O5And Ni2O3, prepare Zn1- xNixZrNb2O8(0 ＜ x >=0.08) microwave-medium ceramics.Specific embodiment is as follows.
Comparative example
1. according to microwave-medium ceramics component Zn1-xNixZrNb2O8(x=0) ZnO-3.4603g, ZrO, are claimed2- 5.2387g, Nb2O5- 11.3010g dispensings, common 20g；Mixed powder is added in ball grinder, is added after 160ml deionized waters and 150g zirconium balls, Ball milling 8 hours on planetary ball mill, drum's speed of rotation is 1000 revs/min；
Dried 2. the raw material after ball milling is placed in 110 DEG C of baking ovens, cross 40 mesh sieves, obtain evengranular powder；
3. evengranular powder is calcined 2 hours in 1075 DEG C；
4. the powder after calcining is put into ball grinder, deionized water and zirconia ball, materials are added：Absolute ethyl alcohol：Mill Ball=1：16：15, secondary ball milling 8 hours, oven for drying crosses 40 mesh sieves；Then 8% adhesive is added as being granulated, and Cross 80 mesh sieves；A diameter of 10mm is pressed into 8Mpa pressure with powder compressing machine again, thickness is 5mm base substrate；
5. by 1250 DEG C of sintering of base substrate, 8 hours are incubated, higher figure of merit zinc zirconium niobium series microwave dielectric ceramic is made；
Finally, the microwave property (referring to table 1) of resulting product is tested by Network Analyzer and dependence test fixture.
Embodiment 1
1. according to microwave-medium ceramics component Zn1-xNixZrNb2O8(x=0.02) ZnO-3.3909g, ZrO, are claimed2- 5.2384g, Nb2O5- 11.3003g, Ni2O3- 0.0703g dispensings, common 20g；Mixed powder is added in ball grinder, adds 160ml After deionized water and 150g zirconium balls, ball milling 8 hours on planetary ball mill, drum's speed of rotation is 1000 revs/min；
Dried 2. the raw material after ball milling is placed in 110 DEG C of baking ovens, cross 40 mesh sieves, obtain evengranular powder；
3. evengranular powder is calcined 2 hours in 1075 DEG C；
4. the powder after calcining is put into ball grinder, deionized water and zirconia ball, materials are added：Absolute ethyl alcohol：Mill Ball=1：16：15, secondary ball milling 8 hours, oven for drying crosses 40 mesh sieves；Then 8% adhesive is added as being granulated, and Cross 80 mesh sieves；A diameter of 10mm is pressed into 8Mpa pressure with powder compressing machine again, thickness is 5mm base substrate；
5. by 1250 DEG C of sintering of base substrate, 8 hours are incubated, higher figure of merit zinc zirconium niobium series microwave dielectric ceramic is made；
Finally, the microwave property (referring to table 1) of resulting product is tested by Network Analyzer and dependence test fixture.
Embodiment 2
1. according to microwave-medium ceramics component Zn1-xNixZrNb2O8(x=0.04) ZnO-3.3215g, ZrO, are claimed2- 5.2381g, Nb2O5- 11.2997g, Ni2O3- 0.1406g dispensings, common 20g；Mixed powder is added in ball grinder, adds 160ml After deionized water and 150g zirconium balls, ball milling 8 hours on planetary ball mill, drum's speed of rotation is 1000 revs/min；
Dried 2. the raw material after ball milling is placed in 110 DEG C of baking ovens, cross 40 mesh sieves, obtain evengranular powder；
3. evengranular powder is calcined 2 hours in 1075 DEG C；
4. the powder after calcining is put into ball grinder, deionized water and zirconia ball, materials are added：Absolute ethyl alcohol：Mill Ball=1：16：15, secondary ball milling 8 hours, oven for drying crosses 40 mesh sieves；Then 8% adhesive is added as being granulated, and Cross 80 mesh sieves；A diameter of 10mm is pressed into 8Mpa pressure with powder compressing machine again, thickness is 5mm base substrate；
5. by 1250 DEG C of sintering of base substrate, 8 hours are incubated, higher figure of merit zinc zirconium niobium series microwave dielectric ceramic is made；
Finally, the microwave property (referring to table 1) of resulting product is tested by Network Analyzer and dependence test fixture.
Embodiment 3
1. according to microwave-medium ceramics component Zn1-xNixZrNb2O8(x=0.06) ZnO-3.2521g, ZrO, are claimed2- 5.2379g, Nb2O5- 11.2990g, Ni2O3- 0.2109g dispensings, common 20g；Mixed powder is added in ball grinder, adds 160ml After deionized water and 150g zirconium balls, ball milling 8 hours on planetary ball mill, drum's speed of rotation is 1000 revs/min；
Dried 2. the raw material after ball milling is placed in 110 DEG C of baking ovens, cross 40 mesh sieves, obtain evengranular powder；
3. evengranular powder is calcined 2 hours in 1075 DEG C；
4. the powder after calcining is put into ball grinder, deionized water and zirconia ball, materials are added：Absolute ethyl alcohol：Mill Ball=1：16：15, secondary ball milling 8 hours, oven for drying crosses 40 mesh sieves；Then 8% adhesive is added as being granulated, and Cross 80 mesh sieves；A diameter of 10mm is pressed into 8Mpa pressure with powder compressing machine again, thickness is 5mm base substrate；
5. by 1250 DEG C of sintering of base substrate, 8 hours are incubated, higher figure of merit zinc zirconium niobium series microwave dielectric ceramic is made；
Finally, the microwave property (referring to table 1) of resulting product is tested by Network Analyzer and dependence test fixture.
Embodiment 4
1. according to microwave-medium ceramics component Zn1-xNixZrNb2O8(x=0.08) ZnO-3.1828g, ZrO, are claimed2- 5.2376g, Nb2O5- 11.2984g, Ni2O3- 0.2812g dispensings, common 20g；Mixed powder is added in ball grinder, adds 160ml After deionized water and 150g zirconium balls, ball milling 8 hours on planetary ball mill, drum's speed of rotation is 1000 revs/min；
Dried 2. the raw material after ball milling is placed in 110 DEG C of baking ovens, cross 40 mesh sieves, obtain evengranular powder；
3. evengranular powder is calcined 2 hours in 1075 DEG C；
4. the powder after calcining is put into ball grinder, deionized water and zirconia ball, materials are added：Absolute ethyl alcohol：Mill Ball=1：16：15, secondary ball milling 8 hours, oven for drying crosses 40 mesh sieves；Then 8% adhesive is added as being granulated, and Cross 80 mesh sieves；A diameter of 10mm is pressed into 8Mpa pressure with powder compressing machine again, thickness is 5mm base substrate；
5. by 1250 DEG C of sintering of base substrate, 8 hours are incubated, higher figure of merit zinc zirconium niobium series microwave dielectric ceramic is made；
Finally, the microwave property (referring to table 1) of resulting product is tested by Network Analyzer and dependence test fixture.
The detection method of the embodiment of the present invention is as follows：
(1) by Agilent 8720ES Network Analyzers, made pottery using starting to rob the prepared cylinder of parallel plate method measurement The dielectric constant of ceramic material, is put into ESPEC MC-710F types high/low temperature circulation incubator by test fixture and carries out resonant frequency temperature The measurement of coefficient, temperature range is 25-85 DEG C of test frequency in the range of 9-11GHz.
(2) using the quality factor of the prepared cylindrical ceramic sample of enclosed cell method measurement.
Every key parameter of the specific embodiment of the invention and its testing result of dielectric properties refer to table 1.
Table 1

Claims (7)

1. a kind of high-performance zinc zirconium niobium series microwave dielectric ceramic, consisting of Zn1-xNixZrNb2O8, wherein 0 ＜ x≤0.08.
The preparation method of above-mentioned high-performance zinc zirconium niobium series microwave dielectric ceramic, has steps of：
(1) by raw material ZnO, ZrO2、Nb2O5And Ni2O3, by chemical formula Zn1-xNixZrNb2O8, wherein x=0~0.08 is matched somebody with somebody Material, then powder is put into ball grinder, add deionized water and zirconia ball, ball milling 6~8 hours on ball mill；
(2) powder after step (1) ball milling is placed under 110 DEG C of oven conditions and dried, after after raw material drying, sieved, acquisition The uniform powder of grain；
(3) powder for being well mixed step (2) carries out pre-burning in 1000~1100 DEG C, and burn-in time is 1~4 hour；
(4) ceramic powder after step (3) pre-burning is put into ball grinder, deionized water and zirconia ball is added, in ball mill Upper secondary ball milling 6~8 hours；Additional 8% adhesive is granulated in ceramic powder after air-drying, and crosses 80 mesh sieves, then use powder Tablet press machine is shaped to base substrate；
(5) base substrate of step (4) is incubated 1~8 hour in 1200-1250 DEG C of sintering, the zinc zirconium niobium system of high quality factor is made Microwave-medium ceramics.
2. a kind of high-performance zinc zirconium niobium series microwave dielectric ceramic according to claim 1, it is characterised in that the step (1) raw material ZnO, ZrO2、Nb2O5And Ni2O3Quality purity be more than 99.9%.
3. a kind of high-performance zinc zirconium niobium series microwave dielectric ceramic according to claim 1, it is characterised in that the step (3) calcined temperature is 1075 DEG C.
4. a kind of high-performance zinc zirconium niobium series microwave dielectric ceramic according to claim 1, it is characterised in that the step (1), the mass ratio of the raw material of step (4) ball-milling technology, deionized water and zirconia ball is 2:16:15.
5. a kind of high-performance zinc zirconium niobium series microwave dielectric ceramic according to claim 1, it is characterised in that the step (4) pressure of powder compressing machine is 2~8Mpa.
6. a kind of high-performance zinc zirconium niobium series microwave dielectric ceramic according to claim 1, it is characterised in that the step (4) blank diameter is 10~20mm, and thickness is 2~8mm.
7. a kind of high-performance zinc zirconium niobium series microwave dielectric ceramic according to claim 1, it is characterised in that the step (5) sintering temperature is 1250 DEG C.
CN201610974137.6A 2016-11-04 2016-11-04 A kind of high-performance zinc zirconium niobium series microwave dielectric ceramic Pending CN107056295A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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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