CN103496986B - Low temperature sintered microwave dielectric ceramic BiCa9V7O28 and preparation method thereof - Google Patents
Low temperature sintered microwave dielectric ceramic BiCa9V7O28 and preparation method thereof Download PDFInfo
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- CN103496986B CN103496986B CN201310459009.4A CN201310459009A CN103496986B CN 103496986 B CN103496986 B CN 103496986B CN 201310459009 A CN201310459009 A CN 201310459009A CN 103496986 B CN103496986 B CN 103496986B
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Abstract
The invention discloses a low temperature sintered microwave dielectric ceramic BiCa9V7O28 and a preparation method thereof. The chemical formula of the low temperature sintered microwave dielectric ceramic is BiCa9V7O28. The preparation method comprises the following steps: (1) weighing and mixing original powder, with purity above 99.9%, of Bi2O3, CaCO3 and V2O5 according to the chemical formula BiCa9V7O28; (2) carrying out wet ball milling on the raw material mixture obtained in the step (1) for 12 hours and presintering the powder in an atmosphere at 780 DEG C for 6 hours after drying the powder, wherein the solvent is distilled water; (3) adding a binder to the powder prepared in the step (2) and then granulating the mixture, then carrying out compression forming and finally sintering the product in an atmosphere at 850-880 DEG C for 4 hours, wherein a polyvinyl alcohol solution with mass concentration of 5% is adopted as the binder and the dosage of the binder is 3% of the total mass of the powder. The prepared ceramic is well sintered at 850-880 DEG C, has dielectric constant of 17-18 and quality factor (Qf) as high as 81000-97000GHz, has low temperature coefficient of resonance frequency, can be co-sintered with Ag electrodes at low temperature and has great application value in industry.
Description
Technical field
The present invention relates to dielectric ceramic material, particularly relate to microwave dielectric ceramic material of the microwave devices such as medium substrate, resonator and the filter used in microwave frequency and preparation method thereof.
Background technology
Microwave dielectric ceramic refers to and to be applied in microwave frequency band (mainly UHF, SHF frequency range) circuit as dielectric material and to complete the pottery of one or more functions, the components and parts such as resonator, 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, telstar recipient 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 property 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 dielectric loss tan δ to reduce noise, General Requirements Qf>=3000 GHz; (3) the temperature coefficient τ of resonance frequency
?little of as far as possible to ensure the thermal stability that device has had, General Requirements-10/ DEG C≤τ
?≤+10 ppm/ DEG C.From late 1930s, just someone attempts dielectric substance to be applied to microwave technology in the world.
According to relative dielectric constant ε
rsize from use frequency range different, usually the microwave dielectric ceramic 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
?≤ 10 ppm/ ° 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 hybrid system MWDC material between them.Its ε
r=25 ~ 30, Q=(1 ~ 2) × 10
4(under the GHz of f>=10), τ
?≈ 0.Be mainly used in the microwave communication equipments such as the direct broadcasting satellite of f >=8 GHz 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 ~ 40, Q=(6 ~ 9) × 10
3(under f=3 ~-4GHz), τ
?≤ 5 ppm/ ° C.Be mainly used in microwave military radar in 4 ~ 8 GHz frequency ranges 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 frequency range, 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
3dielectric constant 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 multilayer ceramic capacitor altogether.In recent years, along with LTCC Technology (Low Temperature Co-fired Ceramics, the requirement of development LTCC) and the development of microwave multilayer device, researcher 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 temperature sintering microwave dielectric ceramic of glassy phase.We are to consisting of BiCa
9v
7o
28, BiBa
9v
7o
28and BiSr
9v
7o
28vanadate pottery carried out sintering characteristic and microwave dielectric property is tested, found that BiCa
9v
7o
28at 850-880 DEG C of sintering, and excellent microwave dielectric property can be had; BiBa
9v
7o
28and BiSr
9v
7o
2although 8 sintering temperatures are lower than 960 DEG C, microwave frequency band dielectric loss is large and can not use as microwave dielectric ceramic.
Summary of the invention
The object of this invention is to provide and a kind ofly have low-loss and good thermal stability, sintering temperature is low, microwave dielectric ceramic that can be low temperature co-fired with Ag and preparation method thereof.
The chemical composition of the low temperature sintering microwave dielectric ceramic that the present invention relates to is: BiCa
9v
7o
28.
Preparation method's concrete steps of described low temperature sintering microwave dielectric ceramic are:
(1) be the Bi of more than 99.9% by purity
2o
3, CaCO
3and V
2o
5starting powder press BiCa
9v
7o
28chemical formula weigh batching.
(2) by step (1) raw material mixing wet ball-milling 12 hours, solvent is distilled water, pre-burning 6 hours in 780 DEG C of air atmosphere after oven dry.
(3) in the powder that step (2) is obtained, binding agent is added and after granulation, more compressing, finally in 850 ~ 880 DEG C of air atmosphere, sinter 4 hours; Described binding agent adopts mass concentration to be the poly-vinyl alcohol solution of 5%, and dosage accounts for 3% of powder gross mass.
Pottery prepared by the present invention is good at 850-880 DEG C of sintering, and its dielectric constant reaches 17 ~ 18, and quality factor q f value is up to 81000-97000GHz, and temperature coefficient of resonance frequency is little, can be low temperature co-fired with Ag electrode, industrially has great using value.
Embodiment
Embodiment:
Table 1 shows 4 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.By BiCa
9v
7o
28powder mixes with the Ag powder accounting for powder quality 20%, compressing after, at 880 DEG C sinter 4 hours; X x ray diffraction material phase analysis and scanning electron microscopic observation all show BiCa
9v
7o
28chemical reaction is not there is not, i.e. BiCa with Ag
9v
7o
28can be low temperature co-fired with Ag electrode.
The present invention is never limited to above embodiment.Bound, the interval value of sintering temperature can realize the present invention, do not enumerate embodiment at this.
This pottery can be widely used in the manufacture of the microwave devices such as various medium substrate, resonator and filter, can meet the technology needs of the system such as mobile communication, satellite communication.
Table 1:
Claims (1)
1. vanadate is as can the application of low-temperature sintered microwave dielectric ceramic, it is characterized in that the chemical constitution formula of described vanadate is: BiCa
9v
7o
28;
Preparation method's concrete steps of described vanadate are:
(1) be the Bi of more than 99.9% by purity
2o
3, CaCO
3and V
2o
5starting powder press BiCa
9v
7o
28chemical formula weigh batching;
(2) by step (1) raw material mixing wet ball-milling 12 hours, solvent is distilled water, pre-burning 6 hours in 780 DEG C of air atmosphere after oven dry;
(3) in the powder that step (2) is obtained, binding agent is added and after granulation, more compressing, finally in 850 ~ 880 DEG C of air atmosphere, sinter 4 hours; Described binding agent adopts mass concentration to be the poly-vinyl alcohol solution of 5%, and dosage accounts for 3% of powder gross mass.
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CN104311018B (en) * | 2014-10-12 | 2016-05-18 | 桂林理工大学 | A kind of ultralow dielectric microwave dielectric ceramic and preparation method thereof |
CN104311021B (en) * | 2014-10-13 | 2016-06-29 | 桂林理工大学 | A kind of ultralow dielectric microwave dielectric ceramic and preparation method thereof |
Citations (1)
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---|---|---|---|---|
CN103113103A (en) * | 2013-03-22 | 2013-05-22 | 桂林理工大学 | Low temperature sintered microwave dielectric ceramic BiZn2VO6 and preparation method thereof |
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---|---|---|---|---|
CN103113103A (en) * | 2013-03-22 | 2013-05-22 | 桂林理工大学 | Low temperature sintered microwave dielectric ceramic BiZn2VO6 and preparation method thereof |
Non-Patent Citations (2)
Title |
---|
Ferroelectric and Ionic-Conductive Properties of Nonlinear-Optical Vanadate, Ca9Bi(VO4)7;B.I.Lazoryak et al.;《Chem. Mater.》;20031231(第15期);3003-3010 * |
Synthesis and Structure of ACa9(VO4)7Compounds,A=Bi or a Rare Earth;J.S.O. Evans et al.;《Journal of Solid State Chemistry》;20011231;第157卷;255-260 * |
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