CN108046795A - A kind of adjustable barium-strontium titanate-based Smecta ceramic medium material of high dielectric - Google Patents

A kind of adjustable barium-strontium titanate-based Smecta ceramic medium material of high dielectric Download PDF

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CN108046795A
CN108046795A CN201711471991.1A CN201711471991A CN108046795A CN 108046795 A CN108046795 A CN 108046795A CN 201711471991 A CN201711471991 A CN 201711471991A CN 108046795 A CN108046795 A CN 108046795A
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strontium titanate
smecta
tio
dielectric
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张明伟
辛乐
郭冲
范恒辉
刘志伟
沈世婷
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Shandong University of Technology
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Abstract

A kind of adjustable barium-strontium titanate-based Smecta ceramic medium material of high dielectric, which is characterized in that the component general formula of the high adjustable barium-strontium titanate-based Smecta ceramic medium material of dielectric is：(1‑m%)Ba1‑zSrzTiO3+m%(Sr1‑xBax)2Al2SiO7, wherein, the value range of x is 0≤x≤0.9；The value range of z is 0.4≤z≤0.6；The value range of m is 10wt%≤m%≤90wt%, selects BaCO3Powder, SrCO3Powder, TiO2Powder, SiO2Powder and Al2O3Powder is as primary raw material, according to (1 m%) Ba1‑zSrzTiO3+m%(Sr1‑xBax)2Al2SiO7Dispensing obtains mixed powder through ball milling, drying, high temperature pre-burned, and then, tabletting is burnt till at a temperature of 1200 DEG C ~ 1500 DEG C again through pre-burning at a temperature of 550 DEG C ~ 600 DEG C.The adjustable barium-strontium titanate-based Smecta ceramic medium material of high dielectric produced by the present invention is continuously adjustable in a wide range, and comprehensive performance is high.

Description

A kind of adjustable barium-strontium titanate-based Smecta ceramic medium material of high dielectric
Technical field
The invention belongs to electronic materials and device arts, and in particular to a kind of high dielectric is adjustable barium-strontium titanate-based multiple Close alumino silicate ceramic dielectric material and its preparation.
Background technology
With high-k, low-dielectric loss, nonlinear dielectric constant is adjustable and the adjustable calcium titanium of its Curie temperature Ore deposit structure barium strontium titanate ferroelectric material is in terms of as microwave adjustable device（Such as phase shifter, wave filter, variable condenser and prolong Slow line etc.）Increasingly extensive concern is obtained, is even more the hot spot studied at present especially in terms of as microwave phase shifter.But with Gao Jie The BST ceramic materials of electric constant are difficult to meet itself and driving source internal impedance match and high-power requirement, which greatly limits It is in the application in microwave adjustable device field.QValue is to weigh the major parameter of inductance component,QValue refers to inductor in a certain frequency The ratio between the induction reactance presented when working under the alternating voltage of rate and its equivalent loss resistance.InductorQValue is higher, loss Smaller, efficiency is higher.The dielectric constant of barium strontium titanate BST materials changes with the variation of applying direct current electric field, when voltage is from V (0) when changing to V (app), dielectric constant will generate an increment Deltaεr=[ε r(0)–ε r(app) ], this increment withε r(0)Ratio Percentage becomes adjustability, that is, usesTunability（It is abbreviated as T）= [ε r(0)–ε r(app) ] /ε r(0)× 100% represents.And Apply the light of a particular frequencies simultaneously（Microwave）When will generate corresponding differential phase shift, achieve the purpose that change phase.With this The material of kind characteristic becomes electrooptical material.The ability that phase shifter changes phase angle is mainly determined by adjustability, so high can Tonality is very important for phase shifter material, and therefore, how to prepare both has low-k, heightQValue, Gao Jie The material system of electric tunable characteristic is a technological difficulties, and Ceramic Composite is all that electron ceramic material modification is the most normal all the time With one of with means the most effective, by different quality than Material cladding, enter in various degree with different modes In the lattice structure of crystalline material, cause the change of material microstructure, so as to effectively adjust and improve the correlation of material Energy.In the prior art, researcher uses MgO, MgAl2O6Deng more compound than barium strontium titanate with different quality, development is had The ceramic medium material system of low-k, high q-factor and certain dielectric tunable characteristic.Xiujian Chou of Tongji University etc. People has carried out systematic research to not same amount than barium strontium titanate composite titanic acid magnesium, obtain microwave ceramic dielectric material (ε r=190, Q =189, T=18.1).However, the comprehensive performance of the system needs to further improve.Barium strontium titanate Smecta material The micro-wave dielectric tunable characteristic of material is studied there is not yet relevant report.
The content of the invention
It is an object of the invention to provide a kind of a kind of high adjustable titaniums of dielectric that drawbacks described above, comprehensive performance can be overcome high The preparation method of sour strontium barium base Smecta ceramic medium material, technical solution are：
A kind of adjustable barium-strontium titanate-based Smecta ceramic medium material of high dielectric, high dielectric are adjustable barium-strontium titanate-based The general formula of the component of Smecta ceramic medium material is：(1-m%) Ba1-zSrzTiO3+m%(Sr1-xBax)2Al2SiO7, Wherein, the value range of x is 0≤x≤0.9, the value range that the value range of z is 0.4≤z≤0.6m be 10wt%≤m%≤ 90wt%, its preparation method include the following steps：
（1）Select BaCO3Powder, SrCO3Powder, TiO2Powder, SiO2Powder and Al2O3Powder is as primary raw material, according to (1- m%) Ba1-zSrzTiO3+m%(Sr1-xBax)2Al2SiO7The stoichiometric ratio dispensing of middle Ba, Sr, Ti, Si and Al, the original that will be prepared Material is placed in nylon ball grinder, ball milling is carried out after adding in zirconia ball and ball-milling medium, through 1000 DEG C ~ 1300 after discharging drying DEG C, 2 ~ 4 h pre-burnings and grinding after obtain mixed powder；
（2）It will（1）Described in mixed powder add in zirconia ball and absolute ethyl alcohol or deionized water carry out 20 ~ 24 it is small when ball Mill sieves after discharging drying and mixed powder 2 is made；
（3）It will（2）Described in 2 added weight percentage of mixed powder be 8% ~ 10% polyvinyl alcohol water solution uniformly mix and make Grain, is then pressed into ceramic green piece under 10MPa ~ 100MPa pressure；
（4）It will（3）Described in ceramic green blank at a temperature of 550 DEG C ~ 600 DEG C, when soaking time 4 ~ 10 is small dumping handle It is sintered again when the time at a temperature of 1200 DEG C ~ 1500 DEG C is small for 4 ~ 10 afterwards, it is adjustable barium-strontium titanate-based compound that high dielectric is made Alumino silicate ceramic dielectric material.
The present invention is high, and the adjustable barium-strontium titanate-based Smecta ceramic medium material of dielectric has the following advantages：
（1）The Curie temperature of the ceramic material system can be with Ba/Sr and (1-m%) Ba1-zSrzTiO3+m%(Sr1-xBax)2Al2SiO7（X=0~0.9；Z=0.4~0.6；10 wt%≤m%≤90wt%）Mass ratio is continuously adjustable in a wide range, can To adjust the structure and performance of material system according to the operating temperature requirements of designed adjustable microwave device；
（2）Pass through Ba/Sr and (1-m%) Ba1-zSrzTiO3+m%(Sr1-xBax)2Al2SiO7（X=0~0.9；Z=0.4~0.6；m% The wt% of=10wt%~90）The variation of component ratio, the dielectric constant of ceramic medium material can be continuously adjustable, and it is normal can to obtain dielectric The material system of number seriation, has widened the application range of material；
（3）With heightQValue（Low-dielectric loss）（Q values are up to 462）, low dielectric constant（178）, high adjustable rate（Adjustable rate Up to 21%）, and dielectric constant seriation（I.e.：Dielectric constant can adjust the mass percent of component by changing the numerical value of m And reach the controllability of dielectric constant with variation adjusting Ba, Sr ratio of x, z value）；
（4）Its ingredient is with Ba1-zSrzTiO3Phase and (Sr1-xBax)2Al2SiO7It mutually coexists, there is excellent microwave dielectric property；
（5）Using traditional electronic ceramic technology, simple process and low cost, material system environmental non-toxic side effect, performance It is excellent, suitable for the material of the adjustable microwaves components such as electric tuning microwave resonator, wave filter and microwave-medium antenna.
Specific embodiment
Embodiment 1
（1）According to 70%Ba0.6Sr0.4TiO3+30%Sr2Al2SiO7The stoichiometric ratio of middle Ba, Sr, Ti, Si and Al weigh respectively BaCO311.680g、SrCO313.083g、TiO27.871g 、Al2O32.488g and SiO2The raw material prepared is placed in by 1.484g In nylon ball grinder, ball milling is carried out after adding in zirconia ball and ball-milling medium, after discharging drying respectively through 1000 DEG C, 1300 DEG C, 4 Mixed powder is obtained after h pre-burnings and grinding；
（2）It will（1）Described in mixed powder add in zirconia ball and absolute ethyl alcohol or deionized water carry out 20 it is small when ball milling, go out It sieves after material drying and mixed powder 2 is made；
（3）It will（2）Described in 2 added weight percentage of mixed powder be 8% polyvinyl alcohol water solution uniformly mix and be granulated, Then ceramic green piece is pressed under 10MPa pressure；
（4）It will（3）Described in ceramic green blank at a temperature of 550 DEG C, when soaking time 4 is small dumping processing after, then It is sintered when 4 is small at a temperature of 1200 DEG C, the high adjustable barium-strontium titanate-based Smecta ceramic medium material of dielectric is made,
Experiment BaCO used3Purity is that 99.8%, Alfa Aesar China LTD. are produced, SrCO3Purity is 99.0%, Alfa Aesar China LTD. are produced, TiO2Purity is 99.9%, the high-new inorganic material Co., Ltd production in Foshan, Al2O3It is pure Degree 99.9%, Sinopharm Chemical Reagent Co., Ltd.'s production, SiO2Purity 99.9%, Sinopharm Chemical Reagent Co., Ltd.'s life Production；
The performance of the adjustable barium-strontium titanate-based Smecta ceramic medium material of high dielectric prepared is：Curie temperature Tc （℃）@10kHz are -42, dielectric constantε r（20 DEG C of room temperature）10 kHz of@are 178, dielectric loss tanδ（20 DEG C of room temperature）@10 KHz is 0.0001, dielectric adjustableT（30kV/cm, 20 DEG C）10 kHz of@are 21%, resonant frequency（MHz）For 3370, during resonance Dielectric constantε rFor 163,QIt is worth for 462.
Embodiment 2
（1）According to 50%Ba0.5Sr0.5TiO3+50%(Sr0.92Ba0.08)2Al2SiO7The stoichiometry of middle Ba, Sr, Ti, Si and Al Than weighing BaCO respectively38.376g、SrCO316.278g、TiO25.756g 、Al2O34.058g and SiO22.391g, by what is prepared Raw material is placed in nylon ball grinder, and ball milling is carried out after adding in zirconia ball and ball-milling medium, after discharging drying respectively through 1100 DEG C, Mixed powder is obtained after 1250 DEG C, 4 h pre-burnings and grinding；
（2）It will（1）Described in mixed powder add in zirconia ball and absolute ethyl alcohol or deionized water carry out 21 it is small when ball milling, go out It sieves after material drying and mixed powder 2 is made；
（3）It will（2）Described in 2 added weight percentage of mixed powder be 8.5% polyvinyl alcohol water solution uniformly mix and make Grain, is then pressed into ceramic green piece under 30MPa pressure；
（4）It will（3）Described in ceramic green blank at a temperature of 560 DEG C, when soaking time 6 is small dumping processing after, then It is sintered when 6 is small at a temperature of 1300 DEG C, the high adjustable barium-strontium titanate-based Smecta ceramic medium material of dielectric is made,
Experiment BaCO used3Purity is that 99.8%, Alfa Aesar China LTD. are produced, SrCO3Purity is 99.0%, Alfa Aesar China LTD. are produced, TiO2Purity is 99.9%, the high-new inorganic material Co., Ltd production in Foshan, Al2O3It is pure Degree 99.9%, Sinopharm Chemical Reagent Co., Ltd.'s production, SiO2Purity 99.9%, Sinopharm Chemical Reagent Co., Ltd.'s life Production；
The performance of the adjustable barium-strontium titanate-based Smecta ceramic medium material of high dielectric prepared is：Curie temperature Tc （℃）@10kHz are -60, dielectric constantε r（20 DEG C of room temperature）10 kHz of@are 157, dielectric loss tanδ（20 DEG C of room temperature）@10 KHz is 0.0001, dielectric adjustableT（30kV/cm, 20 DEG C）10 kHz of@are 16%, resonant frequency（MHz）For 2890, during resonance Dielectric constantε rFor 144,QIt is worth for 431.
Embodiment 3
（1）According to 90%Ba0.6Sr0.4TiO3+10%Sr2Al2SiO7The stoichiometric ratio of middle Ba, Sr, Ti, Si and Al weigh respectively BaCO315.017g、SrCO39.972g、TiO210.120g 、Al2O30.829g and SiO2The raw material prepared is placed in by 0.495g In nylon ball grinder, ball milling is carried out after adding in zirconia ball and ball-milling medium, after discharging drying respectively through 1000 DEG C, 1300 DEG C, 2 Mixed powder is obtained after h pre-burnings and grinding；
（2）It will（1）Described in mixed powder add in zirconia ball and absolute ethyl alcohol or deionized water carry out 22 it is small when ball milling, go out It sieves after material drying and mixed powder 2 is made；
（3）It will（2）Described in 2 added weight percentage of mixed powder be 9% polyvinyl alcohol water solution uniformly mix and be granulated, Then ceramic green piece is pressed under 50MPa pressure；
（4）It will（3）Described in ceramic green blank at a temperature of 580 DEG C, when soaking time 8 is small dumping processing after, then It is sintered when 8 is small at a temperature of 1400 DEG C, the high adjustable barium-strontium titanate-based Smecta ceramic medium material of dielectric is made,
Experiment BaCO used3Purity is that 99.8%, Alfa Aesar China LTD. are produced, SrCO3Purity is 99.0%, Alfa Aesar China LTD. are produced, TiO2Purity is 99.9%, the high-new inorganic material Co., Ltd production in Foshan, Al2O3It is pure Degree 99.9%, Sinopharm Chemical Reagent Co., Ltd.'s production, SiO2Purity 99.9%, Sinopharm Chemical Reagent Co., Ltd.'s life Production；
The performance of the adjustable barium-strontium titanate-based Smecta ceramic medium material of high dielectric prepared is：Curie temperature Tc （℃）@10kHz are -7, dielectric constantε r（20 DEG C of room temperature）10 kHz of@are 3521, dielectric loss tanδ（20 DEG C of room temperature）@10 KHz is 0.0007, dielectric adjustableT（30kV/cm, 20 DEG C）10 kHz of@are 35%, resonant frequency（MHz）For 1125, during resonance Dielectric constantε rFor 2631,QIt is worth for 127.
Embodiment 4
（1）According to 10%Ba0.4Sr0.6TiO3+90%(Sr0.1Ba0.9)2Al2SiO7The stoichiometric ratio of middle Ba, Sr, Ti, Si and Al BaCO is weighed respectively323.864g、SrCO33.955g、TiO21.179g 、Al2O36.007g and SiO23.540g, the original that will be prepared Material is placed in nylon ball grinder, and ball milling is carried out after adding in zirconia ball and ball-milling medium, after discharging drying respectively through 1200 DEG C, Mixed powder is obtained after 1250 DEG C, 3 h pre-burnings and grinding；
（2）It will（1）Described in mixed powder add in zirconia ball and absolute ethyl alcohol or deionized water carry out 24 it is small when ball milling, go out It sieves after material drying and mixed powder 2 is made；
（3）It will（2）Described in 2 added weight percentage of mixed powder be 10% polyvinyl alcohol water solution uniformly mix and be granulated, Then ceramic green piece is pressed under 100MPa pressure；
（4）It will（3）Described in ceramic green blank at a temperature of 600 DEG C, when soaking time 10 is small dumping processing after, then It is sintered when 10 is small at a temperature of 1500 DEG C, the high adjustable barium-strontium titanate-based Smecta ceramic medium material of dielectric is made,
Experiment BaCO used3Purity is that 99.8%, Alfa Aesar China LTD. are produced, SrCO3Purity is 99.0%, Alfa Aesar China LTD. are produced, TiO2Purity is 99.9%, the high-new inorganic material Co., Ltd production in Foshan, Al2O3It is pure Degree 99.9%, Sinopharm Chemical Reagent Co., Ltd.'s production, SiO2Purity 99.9%, Sinopharm Chemical Reagent Co., Ltd.'s life Production；
The performance of the adjustable barium-strontium titanate-based Smecta ceramic medium material of high dielectric prepared is：Curie temperature Tc （℃）@10kHz are -47, dielectric constantε r（20 DEG C of room temperature）10 kHz of@are 97, dielectric loss tanδ（20 DEG C of room temperature）@10 kHz For 0.0003, dielectric adjustableT（30kV/cm, 20 DEG C）10 kHz of@are 11%, resonant frequency（MHz）For 1528, dielectric during resonance Constantε rFor 93,QIt is worth for 154.

Claims (1)

1. a kind of adjustable barium-strontium titanate-based Smecta ceramic medium material of high dielectric, which is characterized in that high dielectric can The general formula of component for the barium-strontium titanate-based Smecta ceramic medium material adjusted is：(1-m%) Ba1-zSrzTiO3+m% (Sr1-xBax)2Al2SiO7, wherein, the value range of x is 0≤x≤0.9, and the value range of z is the value of 0.4≤z≤0.6m Scope is 10wt%≤m%≤90wt%, and its preparation method includes the following steps：
Select BaCO3Powder, SrCO3Powder, TiO2Powder, SiO2Powder and Al2O3Powder is as primary raw material, according to (1-m%) Ba1-zSrzTiO3+m%(Sr1-xBax)2Al2SiO7The stoichiometric ratio dispensing of middle Ba, Sr, Ti, Si and Al, the raw material prepared is put In nylon ball grinder, ball milling is carried out after adding in zirconia ball and ball-milling medium, after discharging drying through 1000 DEG C ~ 1300 DEG C, 2 ~ 4 Mixed powder is obtained after h pre-burnings and grinding；
It will（1）Described in mixed powder add in zirconia ball and absolute ethyl alcohol or deionized water carry out 20 ~ 24 it is small when ball milling, go out It sieves after material drying and mixed powder 2 is made；
It will（2）Described in 2 added weight percentage of mixed powder be 8% ~ 10% polyvinyl alcohol water solution uniformly mix and be granulated, Then ceramic green piece is pressed under 10MPa ~ 100MPa pressure；
It will（3）Described in ceramic green blank at a temperature of 550 DEG C ~ 600 DEG C, when soaking time 4 ~ 10 is small dumping processing after It is sintered again when the time at a temperature of 1200 DEG C ~ 1500 DEG C is small for 4 ~ 10, the high adjustable barium-strontium titanate-based comprehensive silicon of dielectric is made Aluminate ceramic medium material.
CN201711471991.1A 2017-12-29 2017-12-29 High-dielectric adjustable barium strontium titanate-based composite aluminosilicate ceramic dielectric material Expired - Fee Related CN108046795B (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
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CN110386816A (en) * 2019-07-23 2019-10-29 山东理工大学 A kind of high adjustable compound gallic acid zinc ceramic material of rate low-loss barium strontium titanate
CN110386815A (en) * 2019-07-23 2019-10-29 山东理工大学 A kind of compound zinc aluminate ceramic material of barium strontium titanate that can be practical with higher adjustable rate low-loss
CN110606738A (en) * 2019-10-17 2019-12-24 湖南湘梅花电子陶瓷有限公司 High-insulation electronic ceramic material and production process thereof
CN115010489A (en) * 2022-05-18 2022-09-06 中国地质大学（武汉） Mineral-based microwave dielectric ceramic material and preparation method and application thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110386816A (en) * 2019-07-23 2019-10-29 山东理工大学 A kind of high adjustable compound gallic acid zinc ceramic material of rate low-loss barium strontium titanate
CN110386815A (en) * 2019-07-23 2019-10-29 山东理工大学 A kind of compound zinc aluminate ceramic material of barium strontium titanate that can be practical with higher adjustable rate low-loss
CN110606738A (en) * 2019-10-17 2019-12-24 湖南湘梅花电子陶瓷有限公司 High-insulation electronic ceramic material and production process thereof
CN115010489A (en) * 2022-05-18 2022-09-06 中国地质大学（武汉） Mineral-based microwave dielectric ceramic material and preparation method and application thereof

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