CN103319177A - Microwave dielectric ceramic Ba3WTiO8 with low-temperature sintering characteristic and preparation method thereof - Google Patents

Abstract

The invention discloses tungstate microwave dielectric ceramic Ba3WTiO8 with a low-temperature sintering characteristic and a preparation method thereof. The composition of the tungstate microwave dielectric ceramic material is Ba3WTiO8. The method comprises the following steps that: firstly, original powder of BaCO3, WO3 and TiO2 with the purity being higher than 99.9 percent is weighed and mixed according to a chemical formula of BaCu2V2O8; secondly, the raw materials are subjected to wet ball milling and mixed for 12 hours, and are pre-sintered for 6 hours in a 600 DEG C atmosphere after being dried, wherein distilled water serves as a solvent; thirdly, after a binder is added for pelleting, compression molding is performed, and finally, sintering is performed for 4 hours in a 1000-1030 DEG C atmosphere, wherein a polyvinyl alcohol solution with the mass concentration of 5 percent is adopted as the binder, and the amount of the binder is 3 percent of the total mass of the powder. The ceramic prepared through the method is properly sintered at 1000 to 1030 DEG C, has the dielectric constant of 17 to 18, the quality factor QF of 75000 to 96000 GHz and a low temperature coefficient of resonance frequency, can be co-fired with Cu electrodes at low temperature, and has great industrial application value.

Description

But low-temperature sintered microwave dielectric ceramic Ba 3wTiO 8and preparation method thereof

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 wave filter that use in microwave frequency and preparation method thereof.

Background technology

Microwave dielectric ceramic refers to and is applied in microwave frequency band (being mainly UHF, SHF frequency range) circuit as dielectric material and completes the pottery of one or more functions, be widely used as the components and parts such as resonator, wave filter, dielectric substrate and medium guided wave loop in modern communication, it is the key foundation material of modern communication technology, at aspects such as portable mobile phone, automobile telephone, cordless telephone, telestar susceptor and military radars, very important application is arranged, in the miniaturization of modern communication instrument, integrated process, just bringing into play increasing effect.

Be applied to the dielectric ceramic of microwave frequency band, should meet the requirement of following dielectric characteristics: (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 are to reduce noise, general requirement Qf>=3000 GHz; (3) the temperature factor τ of resonant frequency _?the as far as possible little thermostability to guarantee that device has had, general requirement-10/ ℃≤τ _?≤+10 ppm/ ℃.From late 1930s, just someone attempts dielectric substance is applied to microwave technology in the world.

According to relative permittivity ε _rsize from use the different of frequency range, usually the microwave-medium ceramics be developed He developing can be divided into to 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 value, be 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=25～30, Q=(1～2) * 10 ⁴(under f>=10 GHz), τ _?≈ 0.Be mainly used in the microwave communication equipments such as direct broadcasting satellite of f >=8 GHz as the dielectric resonance device.

(3) medium ε _rwith the microwave dielectric ceramic of Q value, be mainly with BaTi ₄o ₉, Ba ₂ti ₉o ₂₀(Zr, Sn) TiO ₄deng the MWDC material that is base, its ε _r=35 ~ 40, Q=(6～9) * 10 ³(f=3～-4GHz under), τ _?≤ 5 ppm/ ° C.Be mainly used in the interior microwave military radar of 4～8 GHz range of frequency and communication system as the dielectric resonance device.

(4) high ε _rand the lower microwave dielectric ceramic of Q value is 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 find and have studied perovskite-like tungsten bronze type BaO-Ln in succession 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 above these material systems is generally higher than 1300 ° of C, can not be directly and the low melting point metals such as Ag and Cu burn altogether the formation laminated ceramic capacitor.In recent years, along with LTCC Technology (Low Temperature Co-fired Ceramics, 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 to adopt devitrified glass or glass-ceramic composite system, because low melting glass has relatively high dielectric loss mutually, the existence of glassy phase has improved the dielectric loss of material greatly.Therefore development is the emphasis of current research without the low fired microwave dielectric ceramic material of glassy phase.

Summary of the invention

The purpose of this invention is to provide a kind of have low-loss and good thermostability, tungstate microwave dielectric ceramic material that sintering temperature is low simultaneously and preparation method thereof.

The chemical constitution formula of tungstate microwave dielectric ceramic material of the present invention is: Ba ₃wTiO ₈.

Preparation method's concrete steps of described tungstate ceramics are:

(1) by purity, be the BaCO more than 99.9% ₃, WO ₃and TiO ₂starting powder press Ba ₃wTiO ₈the chemical formula weigh batching.

(2) step (1) raw material wet ball-milling is mixed 12 hours, solvent is distilled water, pre-burning 6 hours in 600 ℃ of air atmosphere after oven dry.

(3) after adding binding agent granulation in the powder made in step (2), then compression moulding, last sintering 4 hours in 1000 ~ 1030 ℃ of air atmosphere; Described binding agent adopts the polyvinyl alcohol solution that mass concentration is 5%, and dosage accounts for 3% of powder total mass.

Pottery prepared by the present invention is good at 650-680 ℃ of sintering, its specific inductivity reaches 17～18, and quality factor q f value is up to 75000-96000GHz, and temperature coefficient of resonance frequency is little, and can be low temperature co-fired with the Cu electrode, therefore industrial great using value arranged.

Embodiment

Embodiment:

Table 1 shows 4 specific embodiments and the microwave dielectric property thereof that forms different sintering temperatures of the present invention.Its preparation method as mentioned above, carries out the evaluation of microwave dielectric property by the cylindrical dielectric resonator method; By powder with the Cu powder that accounts for powder quality 20%, mix, after compression moulding, 1000 ℃ of lower sintering 4 hours; X ray diffraction material phase analysis and scanning electron microscopic observation all show Ba ₃wTiO ₈with Cu, chemical reaction, i.e. Ba do not occur ₃wTiO ₈can be low temperature co-fired with the Cu electrode.

The present invention never is limited to above embodiment.The bound of sintering temperature, interval value can realize the present invention, at this, do not enumerate embodiment.

This pottery can be widely used in the manufacture of the microwave devices such as various medium substrates, resonator and wave filter, can meet the Technology Need of the systems such as mobile communication, satellite communications.

Table 1:

Claims (1)

1. but a tungstate, as the application of low-temperature sintered microwave dielectric ceramic, is characterized in that the chemical constitution formula of described tungstate is: Ba ₃wTiO ₈;

Preparation method's concrete steps of described tungstate are:

(1) by purity, be the BaCO more than 99.9% ₃, WO ₃and TiO ₂starting powder press Ba ₃wTiO ₈the chemical formula weigh batching;

(2) step (1) raw material wet ball-milling is mixed 12 hours, solvent is distilled water, pre-burning 6 hours in 600 ℃ of air atmosphere after oven dry;

(3) after adding binding agent granulation in the powder made in step (2), then compression moulding, last sintering 4 hours in 1000 ~ 1030 ℃ of air atmosphere; Described binding agent adopts the polyvinyl alcohol solution that mass concentration is 5%, and dosage accounts for 3% of powder total mass.