CN105084897A - Ultralow-dielectric-constant microwave dielectric ceramic SmY2V3O12 having near-zero resonance frequency temperature coefficient - Google Patents

Ultralow-dielectric-constant microwave dielectric ceramic SmY2V3O12 having near-zero resonance frequency temperature coefficient Download PDF

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CN105084897A
CN105084897A CN201510563423.9A CN201510563423A CN105084897A CN 105084897 A CN105084897 A CN 105084897A CN 201510563423 A CN201510563423 A CN 201510563423A CN 105084897 A CN105084897 A CN 105084897A
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dielectric
dielectric ceramic
ceramic
microwave dielectric
smy2v3o12
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方亮
唐莹
方维双
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Guilin University of Technology
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Guilin University of Technology
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Abstract

The invention discloses ultralow-dielectric-constant microwave dielectric ceramic SmY2V3O12 having a near-zero resonance frequency temperature coefficient and adopting a tetragonal zirconia structure as well as a preparation method of the microwave dielectric ceramic SmY2V3O12. The method comprises steps as follows: (1) original Sm2O3, Y2O3 and V2O5 powder with the purity higher than 99.9% (weight percentage) is weighed and prepared according to composition of the SmY2V3O12; (2) the raw material in Step (1) is subjected to wet ball milling and mixing for 12 h, distilled water serves as a ball milling medium, and pre-sintering is performed in the atmosphere at the temperature of 800 DEG C for 6 h after drying; (3) a binder is added to powder obtained in Step (2), granulation and compression molding are performed, and finally, sintering is performed in the atmosphere at the temperature of 850-900 DEG C for 4 h, wherein a polyvinyl alcohol solution with the mass concentration of 5% serves as the binder and the adding amount of polyvinyl alcohol accounts for 3% of the total mass of the powder. The prepared ceramic is well sintered at the temperature lower than 900 DEG C, the dielectric constant is 10.7-11.4, the Qf (quality factor) value is up to 145000-193000 GHz, the resonance frequency temperature coefficient is low, and the ceramic has the great industrial application value.

Description

The ultralow dielectric microwave dielectric ceramic SmY of temperature coefficient of resonance frequency nearly zero 2v 3o 12
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.
Summary of the invention
The object of this invention is to provide and a kind of there is good thermostability and low-loss, simultaneously low temperature sintering ultralow dielectric microwave dielectric ceramic material and preparation method thereof.
The chemical constitution of microwave dielectric ceramic material of the present invention is SmY 2v 3o 12.
Preparation method's step of this microwave dielectric ceramic material is:
(1) be 99.9%(weight percent by purity) more than Sm 2o 3, Y 2o 3and V 2o 5starting powder press SmY 2v 3o 12composition weigh batching.
(2) step (1) raw material wet ball-milling is mixed 12 hours, ball-milling medium is distilled water, pre-burning 6 hours in 800 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 850 ~ 900 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: SmY 2v 3o 12ceramic sintering temperature is low, and raw materials cost is low; Specific inductivity reaches 10.7 ~ 11.4, its temperature coefficient of resonance frequency τ ?nearly zero, temperature stability is good; Quality factor q f value, up to 145000-193000GHz, 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 tetragonal zircite structure 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. a tetragonal zircite structure ultralow dielectric microwave dielectric ceramic for temperature coefficient of resonance frequency nearly zero, is characterized in that the chemical constitution of described microwave dielectric ceramic is: SmY 2v 3o 12;
Preparation method's concrete steps of described microwave dielectric ceramic are:
(1) be 99.9%(weight percent by purity) more than Sm 2o 3, Y 2o 3and V 2o 5starting powder press SmY 2v 3o 12composition weigh batching;
(2) step (1) raw material wet ball-milling is mixed 12 hours, ball-milling medium is distilled water, pre-burning 6 hours in 800 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 850 ~ 900 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.
CN201510563423.9A 2015-09-08 2015-09-08 Ultralow-dielectric-constant microwave dielectric ceramic SmY2V3O12 having near-zero resonance frequency temperature coefficient Pending CN105084897A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103319176A (en) * 2013-06-24 2013-09-25 桂林理工大学 Microwave dielectric ceramic BaCu2V2O8 with low temperature sintering function and preparation method thereof
CN104003722A (en) * 2014-05-24 2014-08-27 桂林理工大学 Ultralow-dielectric constant microwave dielectric ceramic Li3AlV2O8 capable of being sintered at low temperature and preparation method thereof
CN104671785A (en) * 2015-02-03 2015-06-03 桂林理工大学 Stable-temperature type microwave dielectric ceramic LaEuW<2>O<9> with high-quality factor and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103319176A (en) * 2013-06-24 2013-09-25 桂林理工大学 Microwave dielectric ceramic BaCu2V2O8 with low temperature sintering function and preparation method thereof
CN104003722A (en) * 2014-05-24 2014-08-27 桂林理工大学 Ultralow-dielectric constant microwave dielectric ceramic Li3AlV2O8 capable of being sintered at low temperature and preparation method thereof
CN104671785A (en) * 2015-02-03 2015-06-03 桂林理工大学 Stable-temperature type microwave dielectric ceramic LaEuW<2>O<9> with high-quality factor and preparation method thereof

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Application publication date: 20151125