CN103964841B - A kind of microwave-tuned composite ceramic material and preparation method thereof - Google Patents

A kind of microwave-tuned composite ceramic material and preparation method thereof Download PDF

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CN103964841B
CN103964841B CN201410162542.9A CN201410162542A CN103964841B CN 103964841 B CN103964841 B CN 103964841B CN 201410162542 A CN201410162542 A CN 201410162542A CN 103964841 B CN103964841 B CN 103964841B
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microwave
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ceramic material
composite ceramic
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CN103964841A (en
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徐业彬
何艳艳
李长年
何卓
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Huazhong University of Science and Technology
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Abstract

The invention discloses a kind of microwave-tuned composite ceramic material and preparation method thereof.This material is by Ba 1-xsr xtiO 3form with mixture, Ba 1-xsr xtiO 3mass percent be 30% ~ 95%, x=0.4 ~ 0.6, mixture is by Mg 3b 2o 6form with MgO, Mg 3b 2o 6mass percentage content is in the mixture 30% ~ 90%.This dielectric material loss is low, and tuning rate is high.Preparation method comprises: preparation Ba 1-xsr xtiO 3and Mg 3b 2o 6powder; At Ba 1-xsr xtiO 3pulverous Mg is mixed in powder 3b 2o 6and MgO, wet ball grinding post-drying; Add PVA granulation, compression moulding green compact; By green compact 400 ~ 800 DEG C of insulations 2 ~ 4 hours, get rid of the organic substance in green compact; Sintering obtains microwave-tuned composite ceramic material.Preparation technology is simple, and cost is low.

Description

A kind of microwave-tuned composite ceramic material and preparation method thereof
Technical field
The invention belongs to microwave ceramic material technical field, more specifically, relate to a kind of microwave-tuned composite ceramic material and preparation method thereof.
Background technology
The microwave devices such as adjustable filter, retarding line, phase shifter, vibrator, syntonizer and phased array antenna are the important devices of field of microwave communication, but too high cost limits its commercial applications widely.Low cost tunable technology will cause the revolution of microwave component and sky thread industrial.
The specific inductivity of microwave-tuned material can change with impressed voltage.Be applied to microwave communication field, the operating frequency of element is changed by impressed voltage, as a wave filter can be allowed to produce frequency agility, this is extremely important to the broadband communications in future, because can realize several user like this at a common frequency range transmission and received signal.The speed of phased array antenna, precision and reliability are all high than corresponding mechanical handling antenna, and the tuning material of novel microwave can reduce the cost of phased array antenna greatly, by make the application of phased array antenna by current military extend to civilian.
In addition, microwave-tuned material also can be used for manufacturing phase shifter.Current phase shifter is ferrite phase shifter and semiconductor diode phase shifter mainly.But in high frequency, PIN diode exists that loss is large, and power is low, needs logical circuit control phase to move, can not the shortcoming such as continuous tuning; Ferrite is low in more than 3GHz loss, and power is large, but its tuning circuit is expensive, and volume is large, heavy, and power consumption is large, only for military field; In addition, the loss ratio of ferrite when 1 ~ 2GHz is large when 10GHz, is not suitable for cell phone and person-to-person communication service; Ferrite phase shifter is difficult to make two dimensional structure.
The specific inductivity of strontium-barium titanate can change with extra electric field, is a kind of suitable microwave-tuned material.Strontium-barium titanate can be applied to various antenna, but the microwave dielectric loss of strontium-barium titanate is too high, needs to improve material.In addition, too large specific inductivity can cause too large insertion loss, with Circuit Matching difficulty.Therefore, how to obtain and there is moderate specific inductivity and be technological difficulties compared with the strontium-barium titanate of high tuning rate.
Strontium-barium titanate Ba 1-xsr xtiO 3can reduce specific inductivity, dielectric loss with linear dielectric materials compound, and tuning rate remains on higher scope, wherein with Ba 1-xsr xtiO 3the over-all properties of-MgO is best.But for reducing the dielectric loss of composite ceramics, usually need to increase linear medium as the content of MgO, result causes the reduction of tuning rate, and for microwave-tuned application, wishes that tuning rate is more high better.If while the dielectric loss reducing composite ceramics, the tuning rate of composite ceramics can also be improved, will be favourable to microwave-tuned application.
Summary of the invention
For above defect or the Improvement requirement of prior art, the invention provides a kind of microwave-tuned composite ceramic material and preparation method thereof.This material dielectric constant is moderate, and dielectric loss is low, and tuning rate is high, is particularly useful for microwave tuning components.Preparation technology is simple, and cost is low, can sinter within the scope of 1050 DEG C ~ 1200 DEG C, and obtained composite ceramic material composition is with Ba 1-xsr xtiO 3, Mg 3b 2o 6exist with MgO three-phase composite thing, there is no impurity phase.
For achieving the above object, according to one aspect of the present invention, provide a kind of microwave-tuned composite ceramic material, it is characterized in that, it is by Ba 1-xsr xtiO 3form with mixture, wherein, Ba 1-xsr xtiO 3mass percent be 30% ~ 95%, x=0.4 ~ 0.6, described mixture is by Mg 3b 2o 6form with MgO, wherein, Mg 3b 2o 6mass percentage content is in the mixture 30% ~ 90%.
According to another aspect of the present invention, provide a kind of preparation method of above-mentioned microwave-tuned composite ceramic material, it is characterized in that, comprise the steps:
(1) Ba is prepared 1-xsr xtiO 3and Mg 3b 2o 6powder;
(2) according to proportioning at Ba 1-xsr xtiO 3pulverous Mg is mixed in powder 3b 2o 6and MgO, wet ball grinding 6 ~ 24 hours post-dryings;
(3) polyvinyl alcohol (PVA) granulation of 3 ~ 8wt% is added in material after the drying, then compression moulding green compact;
(4) green compact are heated to 400 DEG C ~ 800 DEG C, heat-up rate is less than or equal to 30 DEG C/min, is then incubated 2 ~ 4 hours, gets rid of the organic substance in green compact;
(5) sinter within the scope of 1050 DEG C ~ 1200 DEG C, then be incubated 2 ~ 4 hours, obtain microwave-tuned composite ceramic material.
Preferably, described step (1) is specially: with pulverous BaCO 3, SrCO 3and TiO 2be mixed in proportion as one group of raw material, with pulverous H 3bO 3be mixed in proportion as another group raw material with MgO, by two groups of raw materials wet ball grindings 6 ~ 24 hours respectively, then discharging, oven dry, then pre-burning 2 ~ 6 hours within the scope of 1000 DEG C ~ 1300 DEG C, obtain Ba respectively 1-xsr xtiO 3and Mg 3b 2o 6powder.
In general, the above technical scheme conceived by the present invention compared with prior art, has following beneficial effect:
1, by material prescription of the present invention, can sinter within the scope of 1050 DEG C ~ 1200 DEG C, and this material to have specific inductivity moderate, dielectric loss is low, and tuning rate height waits excellent properties, achieves the result that high-performance and sintering temperature and low have both simultaneously.
2, by regulating the Mg in component 3b 2o 6with the doping of MgO, Mg 3b 2o 6with content ratio and the Sr/Ba ratio of MgO, change the Curie temperature of material, the dependent dielectric performance of adjustment and design composite ceramic material, especially specific inductivity, dielectric loss and tuning rate etc., widened the range of application of material.
3, preparation technology is simple, and cost is low, material system environmental non-toxic side effect, and obtained composite ceramic material composition is with Ba 1-xsr xtiO 3, Mg 3b 2o 6exist with MgO three-phase composite thing, there is no impurity phase.
4, composite ceramic material of the present invention can be widely used in the adjustable microwave devices such as variable condenser, adjustable filter, phase shifter, variable delay line, voltage-controlled vibrator, adjustable dielectric resonator, adjustable impedance coupling device.Wherein, phase shifter is the important devices of phased array antenna, and directly determine cost and the performance of phased array antenna, this material can replace ferrite expensive in phased array antenna, makes phased array antenna volume less, and quality is lighter, and price is cheaper.
Accompanying drawing explanation
Fig. 1 is the XRD spectrum of the composite ceramic material that embodiment 1 ~ 5 obtains;
Fig. 2 is the Ba that embodiment 1 ~ 5 obtains 0.5sr 0.5tiO 3-MgO-Mg 3b 2o 6the specific inductivity of composite ceramics under 10kHz frequency and the change of dielectric loss;
Fig. 3 is the Ba that embodiment 1 ~ 5 obtains 0.5sr 0.5tiO 3-MgO-Mg 3b 2o 6the tuning rate of composite ceramics under 10kHz frequency, different DC electric field intensity.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.In addition, if below in described each embodiment of the present invention involved technical characteristic do not form conflict each other and just can mutually combine.
The microwave-tuned composite ceramic material of the embodiment of the present invention is by Ba 1-xsr xtiO 3form with mixture, wherein, Ba 1-xsr xtiO 3mass percent be 30% ~ 95%, x=0.4 ~ 0.6, mixture is by Mg 3b 2o 6form with MgO, wherein, Mg 3b 2o 6mass percentage content is in the mixture 30% ~ 90%.
The preparation method of above-mentioned microwave-tuned composite ceramic material comprises the steps:
(1) Ba is prepared 1-xsr xtiO 3and Mg 3b 2o 6powder:
With pulverous BaCO 3, SrCO 3and TiO 2be mixed in proportion as one group of raw material, with pulverous H 3bO 3be mixed in proportion as another group raw material with MgO, by two groups of raw materials wet ball grindings 6 ~ 24 hours respectively, then discharging, oven dry, then pre-burning 2 ~ 6 hours within the scope of 1000 DEG C ~ 1300 DEG C, obtain Ba respectively 1-xsr xtiO 3and Mg 3b 2o 6powder;
(2) according to proportioning at Ba 1-xsr xtiO 3pulverous Mg is mixed in powder 3b 2o 6and MgO, wet ball grinding 6 ~ 24 hours post-dryings;
(3) polyvinyl alcohol (PVA) granulation of 3 ~ 8wt% is added in material after the drying, then compression moulding green compact;
(4) green compact are heated to 400 DEG C ~ 800 DEG C, heat-up rate is less than or equal to 30 DEG C/min, is then incubated 2 ~ 4 hours, gets rid of the organic substance in green compact;
(5) sinter within the scope of 1050 DEG C ~ 1200 DEG C, then be incubated 2 ~ 4 hours, obtain microwave-tuned composite ceramic material.
For making those skilled in the art understand the present invention better, below in conjunction with specific embodiment, the preparation method of microwave-tuned composite ceramic material of the present invention is described in detail.
Embodiment 1 ~ 5
Stoichiometrically prepare Ba respectively 0.5sr 0.5tiO 3and Mg (x=0.5) 3b 2o 6.Particularly, by pulverous BaCO 3, SrCO 3and TiO 2be mixed in proportion as one group of raw material, by pulverous H 3bO 3be mixed in proportion as another group raw material with MgO, respectively to adding dehydrated alcohol or deionized water in raw material, with agate ball or zirconium dioxide for ball-milling medium, after wet ball grinding 6h, discharging, oven dry, powder pre-burning 2 hours at 1100 DEG C, obtains Ba respectively 0.5sr 0.5tiO 3and Mg 3b 2o 6powder.Fixing Ba 0.5sr 0.5tiO 3mass percent be 50%, residue 50% is Mg 3b 2o 6with MgO mixture, in mixture, the mass percent of MgO is respectively 10%, 20%, 40%, 50% and 60%, and remaining composition is Mg 3b 2o 6, corresponding embodiment 1 ~ 5, as shown in table 1 respectively.By formula by Ba 0.5sr 0.5tiO 3, Mg 3b 2o 6with MgO mixing, wet ball grinding 6 hours, discharging, oven dry, adopt the polyvinyl alcohol of 5wt% as tackiness agent granulation, under the pressure of 150MPa, pressed by powder is shaping.After 600 DEG C of binder removal process, in air atmosphere, sinter 3 hours in 1090 DEG C, obtain Ba 0.5sr 0.5tiO 3-MgO-Mg 3b 2o 6composite ceramics.Sample after burning till is processed through fine grinding, after ultrasonic cleaning, upper silver electrode, can be used for dielectric properties test.
The mass percentage of each component in the microwave-tuned composite ceramic material that table 1 is obtained
Embodiment Ba 0.5Sr 0.5TiO 3（%） MgO（%） Mg 3B 2O 6（%）
Embodiment 1 50 5 45
Embodiment 2 50 10 40
Embodiment 3 50 20 30
Embodiment 4 50 25 25
Embodiment 5 50 30 20
As shown in Figure 1, this material is by Ba for the XRD spectrum of the composite ceramic material that embodiment 1 ~ 5 is obtained 0.5sr 0.5tiO 3, MgO and Mg 3b 2o 6three phase composites, do not have other impurity phases.The Ba that embodiment 1 ~ 5 is obtained 0.5sr 0.5tiO 3-MgO-Mg 3b 2o 6the specific inductivity under 10kHz frequency of composite ceramics and dielectric loss are as shown in Figure 2.The Ba that embodiment 1 ~ 5 is obtained 0.5sr 0.5tiO 3-MgO-Mg 3b 2o 6the tuning rate of composite ceramics under 10kHz frequency, different DC electric field intensity as shown in Figure 3.It can thus be appreciated that, increase the mass percent of MgO and reduce Mg 3b 2o 6mass percent, can Ba be made 0.5sr 0.5tiO 3-MgO-Mg 3b 2o 6the specific inductivity of composite ceramics slightly increases, and dielectric loss is tending towards reducing, and tuning rate increases.Such as, when MgO mass percent in mixture is increased to 60% from 10%, the tuning rate under 10kHz, 2.4kV/mm is increased to 7.9% from 5.6%.
The obtained composite ceramic material of testing example 1,3 and 5 specific inductivity at microwave frequencies and dielectric loss, and calculate Qf value (=f/ dielectric loss, f is resonant frequency), the specific inductivity of the composite ceramic material that embodiment 1,3 and 5 is obtained is respectively 147.10,161.19 and 164.69, Qf value is respectively 399GHz, 460GHz and 554GHz, and namely composite ceramics dielectric loss at microwave frequencies reduces with the increase of MgO mass percent.Therefore, increase the mass percent of MgO, the microwave dielectric loss of composite ceramics reduces, and tuning rate increases, highly beneficial to microwave-tuned application.This provide the dielectric loss that is reduced material, improve the method for the tuning rate of material simultaneously.
In the prior art, the reduction of ceramic dielectric loss is often with the reduction of tuning rate.The difficult problem that the tuning rate that the invention solves microwave-tuned composite ceramics reduces with the reduction of dielectric loss.By adjustment Sr/Ba ratio, MgO-Mg 3b 2o 6percent mass is MgO/Mg when 3b 2o 6ratio, can obtain the series material of differing dielectric constant and tuning rate.
Embodiment 6:x=0.6, Ba 0.4sr 0.6tiO 3mass percent be 30%, Mg 3b 2o 6mass percent is in the mixture 70%.
Embodiment 7:x=0.45, Ba 0.55sr 0.45tiO 3mass percent be 60%, Mg 3b 2o 6mass percent is in the mixture 30%.
Embodiment 8:x=0.4, Ba 0.6sr 0.4tiO 3mass percent be 95%, Mg 3b 2o 6mass percent is in the mixture 45%.
With the material described in above-described embodiment 6 ~ 8 and stoicheiometry, prepare microwave-tuned composite ceramic material by the following method, the material obtained all can reach technique effect of the present invention.
(1) stoichiometrically Ba is prepared respectively 1-xsr xtiO 3and Mg 3b 2o 6:
With pulverous BaCO 3, SrCO 3and TiO 2be mixed in proportion as one group of raw material, with pulverous H 3bO 3be mixed in proportion as another group raw material, respectively to adding dehydrated alcohol or deionized water in raw material, with agate ball or zirconium dioxide for ball-milling medium with MgO, ball milling is after 6 ~ 24 hours, discharging, oven dry, powder pre-burning 2 ~ 6 hours within the scope of 1000 DEG C ~ 1300 DEG C, obtains Ba respectively 1-xsr xtiO 3and Mg 3b 2o 6powder;
(2) according to composition and ratio, at Ba 1-xsr xtiO 3mg is mixed in powder 3b 2o 6and MgO, add dehydrated alcohol or deionized water, with agate ball or zirconium dioxide for ball-milling medium, ball milling 6 ~ 24 hours;
(3) the polyvinyl alcohol granulation of 3 ~ 8wt% is added in mixture after the drying and compression moulding green compact;
(4) be warming up to less than 800 DEG C, be incubated 2 ~ 4 hours, to get rid of the organic substance in green compact, the heat-up rate of binder removal process is not higher than 30 DEG C/min;
(5) green compact are sintered within the scope of 1050 DEG C ~ 1200 DEG C, be incubated 2 ~ 4 hours, obtain the bulk of required excellent performance.
Those skilled in the art will readily understand; the foregoing is only preferred embodiment of the present invention; not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.

Claims (3)

1. a microwave-tuned composite ceramic material, is characterized in that, it is by Ba 1-xsr xtiO 3form with mixture, wherein, Ba 1-xsr xtiO 3mass percent be 30% ~ 95%, x=0.4 ~ 0.6, described mixture is by Mg 3b 2o 6form with MgO, wherein, Mg 3b 2o 6mass percentage content is in the mixture 30% ~ 90%.
2. a preparation method for microwave-tuned composite ceramic material as claimed in claim 1, is characterized in that, comprises the steps:
(1) Ba is prepared 1-xsr xtiO 3and Mg 3b 2o 6powder;
(2) according to proportioning at Ba 1-xsr xtiO 3pulverous Mg is mixed in powder 3b 2o 6and MgO, wet ball grinding 6 ~ 24 hours post-dryings;
(3) polyvinyl alcohol (PVA) granulation of 3 ~ 8wt% is added in material after the drying, then compression moulding green compact;
(4) green compact are heated to 400 DEG C ~ 800 DEG C, heat-up rate is less than or equal to 30 DEG C/min, is then incubated 2 ~ 4 hours, gets rid of the organic substance in green compact;
(5) sinter within the scope of 1050 DEG C ~ 1200 DEG C, then be incubated 2 ~ 4 hours, obtain microwave-tuned composite ceramic material.
3. the preparation method of microwave-tuned composite ceramic material as claimed in claim 2, it is characterized in that, described step (1) is specially: with pulverous BaCO 3, SrCO 3and TiO 2be mixed in proportion as one group of raw material, with pulverous H 3bO 3be mixed in proportion as another group raw material with MgO, by two groups of raw materials wet ball grindings 6 ~ 24 hours respectively, then discharging, oven dry, then pre-burning 2 ~ 6 hours within the scope of 1000 DEG C ~ 1300 DEG C, obtain Ba respectively 1-xsr xtiO 3and Mg 3b 2o 6powder.
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101723662A (en) * 2009-12-04 2010-06-09 同济大学 Dielectric adjustable BST-MB two-phase compound microwave ceramic material and method for preparing same
CN102992779A (en) * 2012-11-28 2013-03-27 同济大学 2-2 composite structure ceramic material with high-dielectric adjustable and controllable dielectric constant and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101723662A (en) * 2009-12-04 2010-06-09 同济大学 Dielectric adjustable BST-MB two-phase compound microwave ceramic material and method for preparing same
CN102992779A (en) * 2012-11-28 2013-03-27 同济大学 2-2 composite structure ceramic material with high-dielectric adjustable and controllable dielectric constant and preparation method thereof

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