CN105503174A - Temperature-stable low-dielectric-constant microwave dielectric ceramic Bi2LaNbTiO9 and preparation method thereof - Google Patents
Temperature-stable low-dielectric-constant microwave dielectric ceramic Bi2LaNbTiO9 and preparation method thereof Download PDFInfo
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Abstract
The invention discloses temperature-stable low-dielectric-constant microwave dielectric ceramic Bi2LaNbTiO9 and a preparation method thereof. Firstly, chemical raw materials of Bi2O3, La2O3, Nb2O5 and TiO2 powder are weighed and matched according to the stoichiometric equation of Bi2LaNbTiO9; secondly, the raw materials in the first step are mixed for 12 h in a wet ball mill, ball-milling media are distilled water, and pre-sintering is performed in a 900 DEG C atmosphere for 6 h after drying; thirdly, an adhesion agent is added in the powder prepared in the second step, compression molding is performed after pelletizing, and finally, sintering is performed in a 950-980 DEG C atmosphere for 4 h; the adhesion agent is prepared from a polyvinyl alcohol solution with the mass concentration being 5%, and the adding amount of polyvinyl alcohol accounts for 3% of total mass of the powder. The prepared ceramic is good in sintering performance at the temperature of 1000 DEG C, the dielectric constant reaches 33.2-34.5, the quality factor Qf of the ceramic reaches as high as 51900-66100 GHz, the resonance frequency temperature coefficient is small, and the ceramic has great industrial application value.
Description
Technical field
The present invention relates to dielectric ceramic material, particularly relate to dielectric ceramic material of the microwave devices such as ceramic substrate, resonator and the wave filter used for the manufacture of microwave frequency and preparation method thereof.
Background technology
Microwave dielectric ceramic refers to and to be applied in microwave frequency band (mainly UHF and SHF frequency range) circuit as dielectric material and to complete the pottery of one or more functions, the components and parts such as resonator, wave filter, dielectric substrate and medium wave circuit are widely used as in modern communication, it is the key foundation material of modern communication technology, in portable mobile phone, automobile telephone, cordless telephone, telestar susceptor and military radar etc., there is very important application, in the miniaturization, integrated process of modern communication instrument, just playing increasing effect.
Be applied to the dielectric ceramic of microwave frequency band, the requirement of following dielectric characteristics should be met: (1) seriation DIELECTRIC CONSTANT ε
rto adapt to the requirement of different frequency and different application occasion; (2) high quality factor q value or low dielectric loss tan δ to reduce noise, general requirement Qf>=3000GHz; (3) the temperature factor τ of resonant frequency
?little of as far as possible to ensure the thermostability that device has had, general requirement-10ppm/ DEG C≤τ
?≤+10ppm/ DEG C.From late 1930s, just someone attempts dielectric substance to be applied to microwave technology in the world, and prepares TiO
2microwave dielectric filter, but its temperature coefficient of resonance frequency τ
?too greatly cannot be practical.Since the seventies in last century, start the large-scale development to medium ceramic material, according to relative permittivity ε
rsize from use frequency range different, usually the microwave-medium ceramics be developed and developing can be divided into 4 classes.
(1) ultralow dielectric microwave dielectric ceramic, main representative is Al
2o
3-TiO
2, Y
2baCuO
5, MgAl
2o
4and Mg
2siO
4deng, its ε
r≤ 20, quality factor q × f>=50000GHz, τ
?≤ 10ppm/ ° of C.Be mainly used in microwave base plate and high-end microwave device.
(2) low ε
rwith the microwave dielectric ceramic of high q-factor, mainly BaO-MgO-Ta
2o
5, BaO-ZnO-Ta
2o
5or BaO-MgO-Nb
2o
5, BaO-ZnO-Nb
2o
5system or the composite system MWDC material between them.Its ε
r=20 ~ 35, Q=(1 ~ 2) × 10
4(under f>=10GHz), τ
?≈ 0.Be mainly used in the microwave communication equipments such as the direct broadcasting satellite of f >=8GHz as dielectric resonance device.
(3) medium ε
rwith the microwave dielectric ceramic of Q value, mainly with BaTi
4o
9, Ba
2ti
9o
20(Zr, Sn) TiO
4deng the MWDC material for base, its ε
r=35 ~ 45, Q=(6 ~ 9) × 10
3(under f=3 ~-4GHz), τ
?≤ 5ppm/ ° of C.Be mainly used in microwave military radar in 4 ~ 8GHz range of frequency and communication system as dielectric resonance device.
(4) high ε
rand the microwave dielectric ceramic that Q value is lower, be mainly used in civilian mobile communcations system in 0.8 ~ 4GHz range of frequency, this is also the emphasis of microwave dielectric ceramic research.Since the eighties, the people such as Kolar, Kato in succession find and have studied perovskite-like tungsten bronze type BaO-Ln
2o
3-TiO
2series (Ln=La, Sm, Nd or Pr etc. are called for short BLT system), complex perovskite structure CaO-Li
2o-Ln
2o
3-TiO
2series, lead base series material, Ca
1-xln
2x/3tiO
3be contour ε
rmicrowave dielectric ceramic, the wherein BaO-Nd of BLT system
2o
3-TiO
2material dielectric constant reaches 90, lead base series (Pb, Ca) ZrO
3specific inductivity reaches 105.
The sintering temperature of these material systems is generally higher than 1300 ° of C above, can not directly and the low melting point metal such as Ag and Cu burn formation laminated ceramic capacitor altogether.In recent years, along with LTCC Technology (LowTemperatureCo-firedCeramics, the requirement of development LTCC) and the development of microwave multilayer device, researchist both domestic and external has carried out exploring widely and studying to some low fever's system materials, mainly adopt devitrified glass or glassceramic composites system, because low melting glass has relatively high dielectric loss mutually, the existence of glassy phase substantially increases the dielectric loss of material.Therefore development is the emphasis of current research without the low fired microwave dielectric ceramic material of glassy phase.
Can in the process of low fired microwave dielectric ceramic materials in exploration and development of new, the material systems such as the Li based compound that intrinsic sintering temperature is low, Bi based compound, tungstate architecture compound and tellurate architecture compound get the attention and research, but due to three performance index (ε of microwave dielectric ceramic
rwith Qf and τ
?) between be that the relation of mutually restriction is (see document: the restricting relation between microwave dielectric ceramic materials dielectric properties, Zhu Jianhua, Liang Fei, Wang little Hong, Lv Wenzhong, electronic component and material, phase March the 3rd in 2005), meet three performance requriementss and the single-phase microwave-medium ceramics of low temperature sintering is considerably less, mainly their temperature coefficient of resonance frequency is usually excessive or quality factor are on the low side and cannot application request.Current is the summary of experience drawn by great many of experiments to the research major part of microwave-medium ceramics, but complete theory is not had to set forth the relation of microtexture and dielectric properties, therefore, in theory also cannot predict its microwave dielectric property such as temperature coefficient of resonance frequency and quality factor from the composition of compound and structure, which greatly limits the development of low temperature co-fired technology and microwave multilayer device.Explore and low-temperature sintering can have near-zero resonance frequency temperature coefficient (-10ppm/ DEG C≤τ with exploitation simultaneously
?≤+10ppm/ DEG C) be that those skilled in the art thirst for solving always but are difficult to the difficult problem that succeeds all the time with the microwave dielectric ceramic of higher figure of merit.We are to Bi
2laNbTiO
9, Bi
2smNbTiO
9and Bi
2ndNbTiO
9series compound carried out the research of microwave dielectric property, find that their sintering temperature is lower than 1000 DEG C, wherein Bi
2smNbTiO
9loss is too large and cannot find resonance peak, and Bi
2ndNbTiO
9less but the temperature coefficient of resonance frequency (τ bigger than normal of loss
?=69ppm/ DEG C) and cannot as practical microwave-medium ceramics.
Summary of the invention
The object of this invention is to provide the application of a kind of titanate as temperature-stable dielectric constant microwave dielectric ceramic, and prepare the method for this microwave dielectric ceramic.This microwave dielectric ceramic has good thermostability and low-loss, simultaneously can low-temperature sintering.
The chemical constitution of microwave dielectric ceramic material of the present invention is Bi
2laNbTiO
9.
Preparation method's step of this microwave dielectric ceramic material is:
(1) by chemical feedstocks Bi
2o
3, La
2o
3, Nb
2o
5and TiO
2powder is formula Bi stoichiometrically
2laNbTiO
9weigh batching.
(2) step (1) raw material wet ball-milling is mixed 12 hours, ball-milling medium is distilled water, pre-burning 6 hours in 900 DEG C of air atmosphere after oven dry.
(3) in the powder that step (2) is obtained, binding agent is added and after granulation, then compression moulding, finally in 950 ~ 980 DEG C of air atmosphere, sinter 4 hours; Described binding agent adopts mass concentration to be the polyvinyl alcohol solution of 5%, and polyvinyl alcohol addition accounts for 3% of powder total mass.
Advantage of the present invention: Bi
2laNbTiO
9ceramic sintering temperature is low, and raw materials cost is low; Specific inductivity reaches 33.2 ~ 34.5, the temperature factor τ of its resonant frequency
?little, temperature stability is good; Quality factor q f value, up to 51900-66100GHz, can be widely used in the manufacture of the microwave devices such as various medium substrate, resonator and wave filter, can meet the technology needs of low temperature co-fired technology and microwave multilayer device.
Embodiment
Embodiment:
Table 1 shows 3 specific embodiments and microwave dielectric property thereof that form different sintering temperature of the present invention.Its preparation method is described above, carries out the evaluation of microwave dielectric property by cylindrical dielectric resonator method; Adopt X-ray diffraction analysis to carry out material phase analysis, all samples is one-component ceramic.
This pottery can be widely used in the manufacture of the microwave devices such as various medium substrate, resonator and wave filter, can meet the technology needs of the system such as mobile communication and satellite communications.
Table 1:
Claims (1)
1. titanate is as an application for temperature-stable dielectric constant microwave dielectric ceramic, it is characterized in that the chemical constitution of described microwave dielectric ceramic is: Bi
2laNbTiO
9, its specific inductivity is 33.2 ~ 34.5, and temperature coefficient of resonance frequency is 9ppm/ DEG C;
Preparation method's concrete steps of described microwave dielectric ceramic are:
(1) by chemical feedstocks Bi
2o
3, La
2o
3, Nb
2o
5and TiO
2powder is formula Bi stoichiometrically
2laNbTiO
9weigh batching;
(2) step (1) raw material wet ball-milling is mixed 12 hours, ball-milling medium is distilled water, pre-burning 6 hours in 900 DEG C of air atmosphere after oven dry;
(3) in the powder that step (2) is obtained, binding agent is added and after granulation, then compression moulding, finally in 950 ~ 980 DEG C of air atmosphere, sinter 4 hours; Described binding agent adopts mass concentration to be the polyvinyl alcohol solution of 5%, and polyvinyl alcohol addition accounts for 3% of powder total mass.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110845229A (en) * | 2019-11-27 | 2020-02-28 | 中国科学技术大学 | LaBiO3Film, LaBiO3Ceramic target material and preparation method thereof |
CN116063849A (en) * | 2023-02-15 | 2023-05-05 | 哈尔滨理工大学 | High-dielectric composite material and preparation method and application thereof |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103496973A (en) * | 2013-10-07 | 2014-01-08 | 桂林理工大学 | Low temperature sintered microwave dielectric ceramic BiTiNbO6 and preparation method thereof |
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- 2015-12-19 CN CN201510951134.6A patent/CN105503174A/en active Pending
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Publication number | Priority date | Publication date | Assignee | Title |
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CN103496973A (en) * | 2013-10-07 | 2014-01-08 | 桂林理工大学 | Low temperature sintered microwave dielectric ceramic BiTiNbO6 and preparation method thereof |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110845229A (en) * | 2019-11-27 | 2020-02-28 | 中国科学技术大学 | LaBiO3Film, LaBiO3Ceramic target material and preparation method thereof |
CN116063849A (en) * | 2023-02-15 | 2023-05-05 | 哈尔滨理工大学 | High-dielectric composite material and preparation method and application thereof |
CN116063849B (en) * | 2023-02-15 | 2023-08-15 | 哈尔滨理工大学 | High-dielectric composite material and preparation method and application thereof |
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