CN108373330A - Intermediate sintering temperature microwave-medium ceramics and preparation method thereof - Google Patents
Intermediate sintering temperature microwave-medium ceramics and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of intermediate sintering temperature microwave-medium ceramics, synthetic expression formula is：Zn3Nb2‑xSbxO8, wherein x=0.01~0.07.First by ZnO, Nb2O5、Sb2O5Stoichiometrically formula carries out dispensing, by ball milling, drying, sieving, is granulated in 1100 DEG C of calcinings, then additional 0.9%~1.1% polyvinyl alcohol, then pressure forming is green body, and microwave-medium ceramics are made in 1150 DEG C~1210 DEG C sintering in green body.The permittivity ε of the present inventionrIt is 21~22, quality factor q f values are 80350GHz~100881GHz, temperature coefficient of resonance frequency τfIt is 64ppm/ DEG C~70ppm/ DEG C.Due to the presence of not no Ti, reducing atmosphere sintering can be applied to.Present invention process is simple, has saved time and energy cost, and application prospect is extensive.
Description
Technical field
The ceramic composition that the invention belongs to a kind of characterized by ingredient, more particularly to one kind is with Zn3Nb2-xSbxO8To change
The intermediate sintering temperature of formula, the microwave dielectric ceramic materials and preparation method thereof with good microwave dielectric property.
Background technology
There is microwave signal extremely high frequency, extremely short wavelength, big information capacity to have highly directive, penetrability and absorb energy
Power, and microwave equipment can realize the confidentiality of communication, the application being advantageous in field of communication technology and military field.Closely
Field of microwave communication rapidly develops over year.It is led for the microwave communication of representative with satellite communication, automobile telephone and portable phone etc.
Domain constantly proposes the microwave material as communication device and circuit supporting new requirements at the higher level.Microwave-medium ceramics have Gao Jie
The excellent performances such as electric constant, low lossy microwave, temperature coefficient be small are widely used in and make various microwave devices：Microwave oscillator, filter
Wave device and frequency discriminator etc. have incomparable excellent in terms of microwave circuit miniaturization, integrated, high reliability and low cost
Gesture.
Multi-layer ceramics cofiring technology is a kind of new device packaged type developed in recent years.It is by ceramic powder
The accurate and fine and close green band of thickness is made, is printed using laser boring, micropore slip casting, accurate conductor paste on green band
Etc. techniques make required circuitous pattern, then overlap together, by suitable inside and outside metal electrode such as Ni, Ag, Cu etc.,
Different devices is connected in an appropriate manner, the non-interfering high-density circuit of three dimensions is made.And then with it is passive/
The mode of active integrated function module, by circuit miniaturization and densification.With multilayerceramic device the number of plies it is continuous
Increase, the cost of metal paste and electrode already takes up the overwhelming majority of device cost, seriously constrains the production application of device.
In view of electric conductivity and cost, the electrodes in base metal such as Ni, Cu become first choice.However Ni, Cu electrode are easy to oxygen in high temperature sintering
Change, needs to be sintered using reducing atmosphere.The system containing valence variation element such as titanate, has been reduced under reducing atmosphere, and produces
Raw Lacking oxygen, leads to the drastically deterioration of dielectric properties.Therefore, the new microwave-medium system without containing valence variation element is found, with
The application demand for meeting base metal low cost becomes the hot spot of research.
Invention content
The purpose of the present invention is the microwave-medium system without containing valence variation element to find new, reducing atmosphere is suitble to burn
Knot provides one kind with ZnO, Nb to meet the application demand of base metal low cost2O5、Sb2O5For raw material, using conventional solid
Method prepares a kind of class niobates structure Zn with good microwave dielectric property3Nb2-xSbxO8Microwave-medium ceramics.The material by
In the presence of not Ti, reducing atmosphere sintering can be applied to.
The present invention is achieved by following technical solution.
A kind of intermediate sintering temperature microwave-medium ceramics, synthetic expression formula are：Zn3Nb2-xSbxO8, wherein x=0.01~
0.07。
The preparation method of the intermediate sintering temperature microwave-medium ceramics, specific implementation step are as follows：
(1) by ZnO, Nb2O5、Sb2O5Stoichiometrically formula Zn3Nb2-xSbxO8, the progress dispensings of wherein x=0.01~0.07；
Powder is put into polyester tank, after deionized water or absolute ethyl alcohol and zirconia ball is added, ball milling 6 hours；
(2) raw material after step (1) ball milling is put into infrared drying oven, in 80~120 DEG C of drying, then crosses 40 mesh
Sieve；
(3) powder after sieving is put into moderate oven, is calcined 4 hours in 1100 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, zirconia ball and deionized water or absolute ethyl alcohol is added, ball milling is after 12 hours
Drying crosses 80 mesh sieve, then is pressed into green body with powder compressing machine with the pressure of 200MPa；
(5) green body of step (4) is kept the temperature 6 hours, intermediate sintering temperature Zn is made in 1150 DEG C~1210 DEG C sintering3Nb2- xSbxO8The wherein microwave-medium ceramics of x=0.01~0.07.
The step (1) carries out ball milling using planetary ball mill, and drum's speed of rotation is 400 revs/min.
The powder of the step (1) is 1 ︰, 10 ︰ 6 with deionized water or the mass ratio of absolute ethyl alcohol and zirconia ball.
The blank diameter of the step (4) is 10mm, thickness 5mm.
The sintering temperature of the step (5) is 1190 DEG C.
The present invention prepares a kind of microwave-medium ceramics material of novel class niobates structure by simple solid-phase synthesis
Expect Zn3Nb2-xSbxO8.Its permittivity εrIt is 21~22, quality factor q f values are 80350GHz~100881GHz, resonant frequency
Temperature coefficient τfIt is -64ppm/ DEG C~-70ppm/ DEG C.Due to the presence of not no Ti, reducing atmosphere sintering can be applied to.This hair
Bright preparation process is simple, using intermediate sintering temperature, saves time cost and energy cost, application prospect are extensive.
Specific implementation mode
The specific embodiment of the invention is as follows：
A kind of intermediate sintering temperature class niobates structure microwave-medium ceramics, synthetic expression formula are：Zn3Nb2-xSbxO8, wherein x
=0.01~0.07.
(1) by ZnO, Nb2O5、Sb2O5Stoichiometrically formula Zn3Nb2-xSbxO8Carry out dispensing；Powder is put into polyester tank
In, deionized water either absolute ethyl alcohol and zirconia ball powder and deionized water or absolute ethyl alcohol and zirconia ball is added
Mass ratio is 1 ︰, 10 ︰ 6, and using planetary ball mill ball milling 6 hours, drum's speed of rotation was 400 revs/min；
(2) raw material after step (1) ball milling is put into infrared drying oven, in 80~120 DEG C of drying, then crosses 40 mesh
Sieve；
(3) powder after drying, sieving is put into moderate oven, is calcined 4 hours in 1100 DEG C；
(4) polyvinyl alcohol that 0.9%~1.1% is added in the powder after step (3) calcining is made as adhesive
Grain, mixed powder is put into ball grinder, zirconia ball and deionized water or absolute ethyl alcohol is added, ball milling is after 12 hours
Drying crosses 80 mesh sieve, then is pressed into green body, blank diameter 10mm with powder compressing machine with the pressure of 200MPa, and thickness is
5mm；
(5) green compact of step (4) are kept the temperature 6 hours, Zn is made in 1150 DEG C~1210 DEG C sintering3Nb2-xSbxO8Microwave
Media ceramic, preferred sintering temperature are 1190 DEG C.
The microwave dielectric property of resulting product is tested by Network Analyzer.
The main technologic parameters and its microwave dielectric property of the specific embodiment of the invention refer to table 1.
Table 1
The invention is not limited in above-described embodiment, the variation of many details is possible, but therefore this does not violate this
The scope and spirit of invention.
Claims (5)
1. a kind of intermediate sintering temperature microwave-medium ceramics, synthetic expression formula are：Zn3Nb2-xSbxO8, wherein x=0.01~0.07.
The preparation method of the intermediate sintering temperature microwave-medium ceramics, specific implementation step are as follows：
(1) by ZnO, Nb2O5、Sb2O5Stoichiometrically formula Zn3Nb2-xSbxO8, the progress dispensings of wherein x=0.01~0.07；By powder
Material is put into polyester tank, after deionized water or absolute ethyl alcohol and zirconia ball is added, ball milling 6 hours；
(2) raw material after step (1) ball milling is put into infrared drying oven, in 80~120 DEG C of drying, then crosses 40 mesh sieve；
(3) powder after sieving is put into moderate oven, is calcined 4 hours in 1100 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, and zirconia ball and deionized water is added or absolute ethyl alcohol, ball milling are dried after 12 hours,
80 mesh sieve is crossed, then green body is pressed into the pressure of 200MPa with powder compressing machine；
(5) green body of step (4) is kept the temperature 6 hours, intermediate sintering temperature Zn is made in 1150 DEG C~1210 DEG C sintering3Nb2-xSbxO8
The wherein microwave-medium ceramics of x=0.01~0.07.
2. intermediate sintering temperature microwave-medium ceramics according to claim 1, which is characterized in that the step (1) uses planet
Formula ball mill carries out ball milling, and drum's speed of rotation is 400 revs/min.
3. intermediate sintering temperature microwave-medium ceramics according to claim 1, which is characterized in that the powder of the step (1) with
The mass ratio of deionized water or absolute ethyl alcohol and zirconia ball is 1 ︰, 10 ︰ 6.
4. intermediate sintering temperature microwave-medium ceramics according to claim 1, which is characterized in that the green body of the step (4) is straight
Diameter is 10mm, thickness 5mm.
5. intermediate sintering temperature microwave-medium ceramics according to claim 1, which is characterized in that the sintering temperature of the step (5)
Degree is 1190 DEG C.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1431166A (en) * | 2003-01-17 | 2003-07-23 | 西安交通大学 | High frequency dielectric ceramic material sintered under low temp and its preparation |
| CN102219500A (en) * | 2011-04-26 | 2011-10-19 | 天津大学 | Medium-temperature sintered magnesium titanate-based microwave dielectric ceramics with high quality factor |
| CN105174949A (en) * | 2015-08-31 | 2015-12-23 | 天津大学 | Low-loss zinc-zirconium-niobium microwave dielectric ceramic |
-
2018
- 2018-01-19 CN CN201810055448.1A patent/CN108373330A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1431166A (en) * | 2003-01-17 | 2003-07-23 | 西安交通大学 | High frequency dielectric ceramic material sintered under low temp and its preparation |
| CN102219500A (en) * | 2011-04-26 | 2011-10-19 | 天津大学 | Medium-temperature sintered magnesium titanate-based microwave dielectric ceramics with high quality factor |
| CN105174949A (en) * | 2015-08-31 | 2015-12-23 | 天津大学 | Low-loss zinc-zirconium-niobium microwave dielectric ceramic |
Non-Patent Citations (2)
| Title |
|---|
| PING ZHANG ET AL.: "Bond ionicity, lattice energy, bond energy and microwave dielectric properties of ZnZr(Nb1−xAx)2O8 (A = Ta, Sb) ceramics", 《DALTON TRANSACTIONS》 * |
| YONGGUI ZHAO ET AL.: "Influence of Ta substitution for Nb in Zn3Nb2O8 and the impact on the crystal structure and microwave dielectric properties", 《DALTON TRANSACTIONS》 * |
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