CN110386815A - A kind of compound zinc aluminate ceramic material of barium strontium titanate that can be practical with higher adjustable rate low-loss - Google Patents
A kind of compound zinc aluminate ceramic material of barium strontium titanate that can be practical with higher adjustable rate low-loss Download PDFInfo
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- C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
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- C04B35/468—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates based on barium titanates
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Abstract
A kind of ferroelectric dielectric materials of the adjustable low-loss barium-strontium titanate-based compound zinc aluminate ceramics of high electricity, which is characterized in that the component general formula of the ferroelectric dielectric materials of the high adjustable low-loss barium-strontium titanate-based compound zinc aluminate ceramics of electricity are as follows: (1-x) Ba0.4Sr0.6TiO3‑xZnAl2O4, wherein the value range of x is the wt% of 30wt%≤x≤70, selects BaTiO3Powder, SrTiO3Powder, ZnO powder and Al2O3Powder is as primary raw material, according to (1-x) Ba0.4Sr0.6TiO3‑xZnAl2O4Ingredient obtains mixed powder by ball milling, drying, high temperature pre-burned, after tabletting at a temperature of 550 DEG C ~ 600 DEG C pre-burning again 1400 DEG C ~ 1450 DEG C at a temperature of be burnt into.The ferroelectric dielectric materials of the high adjustable low-loss barium-strontium titanate-based compound zinc aluminate ceramics of electricity produced by the present invention performance under wide range of operation temperature area is stablized, and comprehensive performance is high.
Description
Technical field
The invention belongs to electronic materials and device arts, and in particular to a kind of high adjustable low-loss barium strontium titanate of electricity
The ferroelectric dielectric materials and its preparation of the compound zinc aluminate ceramics of base.
Background technique
One important feature of ferroelectric material is exactly dielectric, nonlinear, i.e., dielectric constant can become with the variation of extra electric field
Change.This can be applicable to ferroelectric material in microwave device such as tunable oscillator, filter, phase shifter and variodenser.Ferroelectricity material
Expect that barium strontium titanate is one such ideal candidate material, has high adjustable rate, lower dielectric loss and dielectric constant big
The features such as.In addition its Curie temperature can be changed by adjusting Ba/Sr, be at paraelectric phase, this is very beneficial for room temperature
Under work.But barium-strontium titanate ceramic is the problem is that high dielectric constant is difficult to meet itself and driving source internal impedance match
With powerful requirement, which has limited its applications in microwave adjustable device field.Adjustable rate has very strong electric field dependence,
It is represented by Tunablity(and is abbreviated as T)=[ε r(0)–ε r(E) ] /ε r(0)× 100%, whereinε r(0)、ε r(E) Respectively zero electric field
With the dielectric constant of applying direct current off field.Such as typically applying in phase shifter, the ability that device changes phase angle is main
Depending on the adjustability size of material, and if dielectric loss is excessive, device heating can be made serious, therefore the high adjustable low-loss of electricity
Material be us required for.In the performance of material is tailored, adjustable rate, dielectric loss and dielectric constant three are often phase
The relationship mutually restricted, so existing research work is compromised in adjustability, dielectric loss and dielectric constant three's parameter
Regulation, to obtain the optimum performance of device.The compound ferroelectric material of dielectric material always is most simple and efficient method, grinds
Study carefully personnel and find compound low-loss linear dielectric material, the dielectric constant of ferroelectric material can be diluted, to reduce Jie of material
Electrical loss；And the adjustable rate of composite material will receive weakening, the ferroelectric dilution of this and ferroelectric material and linear dielectric material
Redistributing for electric field can be caused related under the electric field.At present it has been reported that ferroelectric dielectric system in, seem BST-MgAl2O4、
BST-Mg2TiO4, dielectric constant, dielectric loss and dielectric adjustable have reached real requirement, but there are still Q values under microwave (to be situated between
The inverse of electrical loss) too low, problem that adjustability is not high enough, there is still a need for further increase for comprehensive performance.
Summary of the invention
A kind of simply high adjustable low-loss metatitanic acid of electricity of high, preparation process that the purpose of the present invention is to provide comprehensive performances
The compound aluminic acid zinc-iron electricity dielectric ceramic material of strontium barium base, technical solution are as follows:
A kind of ferroelectric dielectric materials of the barium-strontium titanate-based compound zinc aluminate ceramics of the high adjustable low-loss of electricity, which is characterized in that high electricity
The chemical constitution formula of adjustable low-loss barium-strontium titanate-based compound zinc aluminate ceramic ferroelectric dielectric material are as follows: (1-x)
Ba0.4Sr0.6TiO3-xZnAl2O4, wherein the value range of x is the 30 wt % of wt %≤x≤70, and preparation method includes
Following steps:
(1) BaTiO is selected3Powder, SrTiO3Powder, ZnO powder and Al2O3Powder is as primary raw material, according to (1-x)
Ba0.4Sr0.6TiO3-xZnAl2O4The raw material prepared is placed in nylon ball by the stoichiometric ratio ingredient of middle Ba, Sr, Ti, Zn and Al
In grinding jar, ball milling is carried out after zirconia ball and ball-milling medium is added, is pre-sintered after discharging drying and is mixed after being ground
Powder 1；It is 1100 DEG C ~ 1200 DEG C in the temperature for carrying out pre-burning, sintering time is 4 ~ 6 hours.
(2) zirconia ball and dehydrated alcohol is added in mixed powder 1 described in (1) or deionized water progress 24 ~ 48 is small
When ball milling, discharging drying after sieving obtain mixed powder 2；
(3) mass ratio is added in mixed powder 2 described in (2) to be uniformly mixed and make for 7% ~ 10% polyvinyl alcohol water solution
Grain, is then pressed into ceramic green piece under 10MPa ~ 100MPa pressure；
(4) by ceramic green blank described in (3) 550 DEG C ~ 600 DEG C at a temperature of, soaking time is at 4 ~ 10 hours dumpings
Reason；The time is to sinter porcelain into 4 ~ 6 hours at 1400 DEG C ~ 1450 DEG C after dumping, and the high adjustable low-loss barium strontium titanate of electricity is made
The ferroelectric dielectric materials of the compound zinc aluminate ceramics of base.
The high adjustable low-loss barium-strontium titanate-based compound aluminic acid zinc-iron electricity dielectric ceramic material of electricity of the invention has following excellent
Point:
(1) by preferred Ba/Sr, the Curie temperature of composite ceramics is controlled in suitable section, composite ceramics (1-x)
Ba0.4Sr0.6TiO3-xZnAl2O4There is high dielectric adjustable in very wide operation temperature area, be particularly suitable for room temperature or more
Operating temperature；
(2) by using different x mass ratioes, dielectric constant is adjusted in suitable different sections, different components can be met
Demand under has widened the application range of material；
(3) (constituent mass is adjusted in the array for changing x with low dielectric constant, low dielectric loss and high electric adjustability
When percentage, can still meet the high-performance of three simultaneously), and the synthesis dielectric properties under microwave are high；
(4) traditional electronic ceramic technology, simple process are used；Material system belongs to green material, nontoxic no pair
Effect.Excellent material performance is suitable for the components such as microwave tunable oscillator, filter, phase shifter and microwave-medium antenna.
Specific embodiment
Embodiment 1
(1) according to 70 wt % Ba0.4Sr0.6TiO3+30 wt % ZnAl2O4In stoichiometric ratio weigh respectively
BaTiO38.4g、SrTiO312.6g, ZnO4g and Al2O3The raw material prepared is placed in nylon ball grinder and oxidation is added by 5g powder
Ball milling is carried out after zirconium ball and ball-milling medium, obtains mixed powder 1 after pre-burning and grinding are carried out after discharging drying；It is carried out in advance described
The temperature of burning is respectively 1100 DEG C and 1200 DEG C, and sintering time is 4 hours；
(2) zirconia ball and dehydrated alcohol is added in mixed powder 1 described in (1) or deionized water carries out ball milling 24 hours,
Sieving obtains mixed powder 2 after discharging drying；
(3) mass ratio is added in mixed powder 2 described in (2) to be uniformly mixed and be granulated for 10% polyvinyl alcohol water solution, so
Ceramic green piece is pressed under 10MPa pressure afterwards；
(4) by ceramic green blank described in (3) 550 DEG C at a temperature of, soaking time is the processing of 10 hours dumpings；After dumping
The time is to sinter porcelain into 4 hours at 1450 DEG C, and the adjustable low-loss barium-strontium titanate-based compound zinc aluminate ceramics of high electricity are made
Ferroelectric dielectric materials.
Experiment BaTiO used3Purity is 99.5%, the production of Mike woods biochemical technology Co., Ltd, SrTiO3Purity is
99.5%, Mike woods biochemical technology Co., Ltd production, ZnO purity is 99.9%, the production of three factory of Tianjin chemical reagent, Al2O3Purity
It is 99.9%, Sinopharm Chemical Reagent Co., Ltd.'s production.The adjustable low-loss barium-strontium titanate-based compound aluminic acid of height electricity of preparation
The ferroelectric dielectric materials performance parameter of zinc ceramics is shown in Table 1.
Embodiment 2
(1) according to 50 wt % Ba0.4Sr0.6TiO3+50 wt % ZnAl2O4In stoichiometric ratio weigh respectively
BaTiO37.0g、SrTiO39.0g, ZnO6.7g and Al2O3The raw material prepared is placed in nylon ball grinder and is added by 8.3g powder
Ball milling is carried out after zirconia ball and ball-milling medium, obtains mixed powder 1 after pre-burning and grinding are carried out after discharging drying；It is described into
The temperature of row pre-burning is respectively 1100 DEG C and 1200 DEG C, and sintering time is 6 hours；
(2) zirconia ball and dehydrated alcohol is added in mixed powder 1 described in (1) or deionized water carries out ball milling 30 hours,
Sieving obtains mixed powder 2 after discharging drying；
(3) mass ratio is added in mixed powder 2 described in (2) to be uniformly mixed and be granulated for 8% polyvinyl alcohol water solution, so
Ceramic green piece is pressed under 30MPa pressure afterwards；
(4) by ceramic green blank described in (3) 580 DEG C at a temperature of, soaking time is the processing of 7 hours dumpings；After dumping
The time is to sinter porcelain into 6 hours at 1400 DEG C, and the adjustable low-loss barium-strontium titanate-based compound zinc aluminate ceramics of high electricity are made
Ferroelectric dielectric materials.
Experiment BaTiO used3Purity is 99.5%, the production of Mike woods biochemical technology Co., Ltd, SrTiO3Purity is
99.5%, Mike woods biochemical technology Co., Ltd production, ZnO purity is 99.9%, the production of three factory of Tianjin chemical reagent, Al2O3Purity
It is 99.9%, Sinopharm Chemical Reagent Co., Ltd.'s production.The adjustable low-loss barium-strontium titanate-based compound aluminic acid of height electricity of preparation
The ferroelectric dielectric materials performance parameter of zinc ceramics is shown in Table 1.
Embodiment 3
(1) according to 30wt % Ba0.4Sr0.6TiO3+70 wt % ZnAl2O4In stoichiometric ratio weigh respectively
BaTiO33.6g、SrTiO35.4g, ZnO9.3g and Al2O3The raw material prepared is placed in nylon ball grinder and is added by 11.7g powder
Ball milling is carried out after zirconia ball and ball-milling medium, obtains mixed powder 1 after pre-burning and grinding are carried out after discharging drying；It is described into
The temperature of row pre-burning is respectively 1200 DEG C and 1200 DEG C, and sintering time is 5 hours；
(2) zirconia ball and dehydrated alcohol is added in mixed powder 1 described in (1) or deionized water carries out ball milling 48 hours,
Sieving obtains mixed powder 2 after discharging drying；
(3) mass ratio is added in mixed powder 2 described in (2) to be uniformly mixed and be granulated for 7% polyvinyl alcohol water solution, so
Ceramic green piece is pressed under 100MPa pressure afterwards；
(4) by ceramic green blank described in (3) 600 DEG C at a temperature of, soaking time is the processing of 4 hours dumpings；After dumping
The time is to sinter porcelain into 5 hours at 1450 DEG C, and the adjustable low-loss barium-strontium titanate-based compound zinc aluminate ceramics of high electricity are made
Ferroelectric dielectric materials.
Experiment BaTiO used3Purity is 99.5%, the production of Mike woods biochemical technology Co., Ltd, SrTiO3Purity is
99.5%, Mike woods biochemical technology Co., Ltd production, ZnO purity is 99.9%, the production of three factory of Tianjin chemical reagent, Al2O3Purity
It is 99.9%, Sinopharm Chemical Reagent Co., Ltd.'s production.The adjustable low-loss barium-strontium titanate-based compound aluminic acid of height electricity of preparation
The ferroelectric dielectric materials performance parameter of zinc ceramics is shown in Table 1.
(1-x) Ba under 1 different composite amount of table and different calcining systems0.4Sr0.6TiO3-xZnAl2O4The electricity of composite material
Performance
The dielectric parameter of composite material is measured by upper table it is found that present complex system comprehensive performance is high: rate that composite material is adjustable
Height, and stability is good (without weakening adjustable rate dielectric constant is greatly reduced)；Dielectric constant is adjusted suitable
Numerical value can satisfy different microwave device demands, while the Q value under microwave has obtained the holding of more excellent degree.Such as in 30 wt
% Ba0.4Sr0.6TiO3+70 wt % ZnAl2O4Compound content under, dielectric constant is adjusted is in 178, dielectric loss
0.0093, and adjustability is up to 31.5%, Q value reaches 707 under microwave.Preparation process of the present invention is simple, and repetitive rate is good and yield rate
Height is suitable for the adjustable component of a variety of microwaves, and is suitble to enterprise scale production.
Claims (1)
1. a kind of ferroelectric dielectric materials of the barium-strontium titanate-based compound zinc aluminate ceramics of the high adjustable low-loss of electricity, which is characterized in that high
The chemical constitution formula of electric adjustable low-loss barium-strontium titanate-based compound zinc aluminate ceramic ferroelectric dielectric material are as follows: (1-x)
Ba0.4Sr0.6TiO3-xZnAl2O4, wherein the value range of x is the 30 wt % of wt %≤x≤70, and preparation method includes
Following steps:
Select BaTiO3Powder, SrTiO3Powder, ZnO powder and Al2O3Powder is as primary raw material, according to (1-x)
Ba0.4Sr0.6TiO3-xZnAl2O4The raw material prepared is placed in nylon ball by the stoichiometric ratio ingredient of middle Ba, Sr, Ti, Zn and Al
In grinding jar, ball milling is carried out after zirconia ball and ball-milling medium is added, is pre-sintered after discharging drying and is mixed after being ground
Powder 1；It is 1100 DEG C ~ 1200 DEG C in the temperature for carrying out pre-burning, sintering time is 4 ~ 6 hours；
Zirconia ball and dehydrated alcohol is added in mixed powder 1 described in (1) or deionized water carries out 24 ~ 48 hours ball millings,
Sieving obtains mixed powder 2 after discharging drying；
Mass ratio is added in mixed powder 2 described in (2) to be uniformly mixed and be granulated for 7% ~ 10% polyvinyl alcohol water solution, so
Ceramic green piece is pressed under 10MPa ~ 100MPa pressure afterwards；
By ceramic green blank described in (3) 550 DEG C ~ 600 DEG C at a temperature of, soaking time is the processing of 4 ~ 10 hours dumpings；
The time is to sinter porcelain into 4 ~ 6 hours at 1400 DEG C ~ 1450 DEG C after dumping, and it is adjustable low-loss barium-strontium titanate-based multiple that high electricity is made
Close the ferroelectric dielectric materials of zinc aluminate ceramics.
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Cited By (3)
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| CN111978080A (en) * | 2020-08-04 | 2020-11-24 | 山东理工大学 | High-adjustable low-loss low-sintering ceramic material of barium strontium titanate composite copper gallate |
| CN118084483A (en) * | 2024-04-29 | 2024-05-28 | 山东理工大学 | BST-based microwave dielectric adjustable composite ceramic material and preparation method thereof |
| CN118084483B (en) * | 2024-04-29 | 2024-07-09 | 山东理工大学 | BST-based microwave dielectric adjustable composite ceramic material and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111978080A (en) * | 2020-08-04 | 2020-11-24 | 山东理工大学 | High-adjustable low-loss low-sintering ceramic material of barium strontium titanate composite copper gallate |
| CN118084483A (en) * | 2024-04-29 | 2024-05-28 | 山东理工大学 | BST-based microwave dielectric adjustable composite ceramic material and preparation method thereof |
| CN118084483B (en) * | 2024-04-29 | 2024-07-09 | 山东理工大学 | BST-based microwave dielectric adjustable composite ceramic material and preparation method thereof |
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