CN104311009B - Temperature-stable dielectric constant microwave dielectric ceramic Sr 2ta 5v 3o 22 - Google Patents

Temperature-stable dielectric constant microwave dielectric ceramic Sr 2ta 5v 3o 22 Download PDF

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CN104311009B
CN104311009B CN201410519070.8A CN201410519070A CN104311009B CN 104311009 B CN104311009 B CN 104311009B CN 201410519070 A CN201410519070 A CN 201410519070A CN 104311009 B CN104311009 B CN 104311009B
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dielectric ceramic
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CN104311009A (en
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王丹
李纯纯
苏和平
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Jiangsu zhuoken Intellectual Property Operation Co.,Ltd.
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Guilin University of Technology
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—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
    • C04B35/495—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 vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
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    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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    • C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins

Abstract

The invention discloses a kind of low temperature sintering temperature-stable dielectric constant microwave dielectric ceramic Sr 2ta 5v 3o 22and preparation method thereof.(1) be 99.9%(weight percent by purity) more than SrCO 3, Ta 2o 5and V 2o 5starting powder press Sr 2ta 5v 3o 22composition 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 820 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 870 ~ 920 DEG C of air atmosphere, sinter 4 hours; Described binding agent adopts mass concentration to be the polyvinyl alcohol solution of 5%, and the addition of polyvinyl alcohol accounts for 3% of powder total mass.Pottery prepared by the present invention is good at 870 ~ 920 DEG C of sintering, and specific inductivity reaches 31.1 ~ 33.3, and its quality factor q f value is up to 49000-68000GHz, and temperature coefficient of resonance frequency is little, industrially has great using value.

Description

Temperature-stable dielectric constant microwave dielectric ceramic Sr 2ta 5v 3o 22
Technical field
The present invention relates to dielectric ceramic material, low dielectric constant dielectric stupalith particularly relating to Ceramic Resonator and the microwave device such as 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=25 ~ 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 production application.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 consisting of Ba 2ta 5v 3o 22, Sr 2ta 5v 3o 22, Ca 2ta 5v 3o 22, Sr 2nb 5v 3o 22vanadate carried out the research of microwave dielectric property, wherein find that their sintering temperature is lower than 950 DEG C, but only have Sr 2ta 5v 3o 22there is near-zero resonance frequency temperature coefficient and high quality factor, the temperature coefficient of resonance frequency (τ all bigger than normal of other composition pottery ?>20ppm/ DEG C).
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 dielectric constant microwave dielectric ceramic material and preparation method thereof.
The chemical constitution of microwave dielectric ceramic material of the present invention is Sr 2ta 5v 3o 22.
Preparation method's step of this microwave dielectric ceramic material is:
(1) be 99.9%(weight percent by purity) more than SrCO 3, Ta 2o 5and V 2o 5starting powder press Sr 2ta 5v 3o 22composition 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 820 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 870 ~ 920 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: ceramic sintering temperature is low, good at 870 ~ 920 DEG C of sintering, specific inductivity reaches 31.1 ~ 33.3, the temperature factor τ of its resonant frequency ?nearly zero, temperature stability is good; Its quality factor q f value, up to 49000-68000GHz, can be widely used in the manufacture of the microwave devices such as various resonator and wave filter, can meet the technology needs of low temperature co-fired technology and microwave multilayer device, industrially have great using value.
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.
This pottery can be widely used in the manufacture of the microwave devices such as various dielectric 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 low temperature sintering temperature-stable dielectric constant microwave dielectric ceramic, is characterized in that the chemical constitution of described microwave dielectric ceramic is: Sr 2ta 5v 3o 22;
Preparation method's concrete steps of described microwave dielectric ceramic are:
(1) be 99.9%(weight percent by purity) more than SrCO 3, Ta 2o 5and V 2o 5starting powder press Sr 2ta 5v 3o 22composition 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 820 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 870 ~ 920 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.
CN201410519070.8A 2014-10-07 2014-10-07 Temperature-stable dielectric constant microwave dielectric ceramic Sr 2ta 5v 3o 22 Active CN104311009B (en)

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