CN104628384B - Low-loss temperature-stabilized medium dielectric constant microwave medium microwave dielectric ceramic LiBi2nbO6 - Google Patents
Low-loss temperature-stabilized medium dielectric constant microwave medium microwave dielectric ceramic LiBi2nbO6 Download PDFInfo
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Abstract
The invention discloses a kind of composite oxides LiBi as the application of low temperature sintering temperature-stable medium dielectric constant microwave medium microwave dielectric ceramic2NbO6And preparation method thereof.(1) be 99.9%(percentage by weight by purity) more than Li2CO3、Bi2O3And Nb2O5Starting powder press LiBi2NbO6Composition weigh dispensing；(2) by step (1) raw material wet ball-milling mix 12 hours, ball-milling medium is dehydrated alcohol, after drying in 850 DEG C of air atmosphere pre-burning 6 hours；(3) after adding binding agent pelletize in the powder that step (2) prepares, re-compacted molding, finally sinter 4 hours in 900 ~ 950 DEG C of air atmosphere；Described binding agent uses mass concentration to be the poly-vinyl alcohol solution of 5%, and the addition of polyvinyl alcohol accounts for the 3% of powder gross mass.Ceramic post sintering prepared by the present invention is good, and dielectric constant reaches 37.3～38.7, and its quality factor q f value is up to 64000 79000GHz, and temperature coefficient of resonance frequency is little, industrially has great using value.
Description
Technical field
The present invention relates to dielectric ceramic material, particularly relate to for manufacturing ceramic substrate, the resonance that microwave frequency uses
Dielectric ceramic materials of microwave device such as device and wave filter and preparation method thereof.
Background technology
Microwave dielectric ceramic refers to be applied in microwave frequency band (mainly UHF and SHF frequency range) circuit as dielectric material
And complete the pottery of one or more functions, modern communication is widely used as resonator, wave filter, dielectric substrate and medium
The components and parts such as wave circuit, are the key foundation materials of modern communication technology, in portable mobile phone, automobile telephone, nothing
The aspect such as rope phone, television satellite accepter and military radar has highly important application, small-sized at modern communication instrument
Change, integrated during just playing increasing effect.
It is applied to the dielectric ceramic of microwave frequency band, should meet the requirement of following dielectric property: (1) seriation DIELECTRIC CONSTANT εr
To adapt to different frequency and the requirement of different application occasion;(2) high quality factor q value or low dielectric loss tan δ are to reduce
Noise, typically requires Qf >=3000 GHz;(3) the temperature coefficient τ of resonant frequencyƒThe least to ensure what device had had
Heat stability, general requirement-10 ppm/DEG C≤τƒ≤+10 ppm/℃.Just have tried to from late 1930s in the world
Dielectric substance is applied to microwave technology, and prepares TiO2Microwave dielectric filter, but its temperature coefficient of resonance frequency τƒ
Too greatly cannot be practical.Since the seventies in last century, the large-scale development to medium ceramic material, root are started
According to relative dielectric constant εrSize from use frequency range different, generally can will have been developed that and developing microwave-medium pottery
Porcelain is divided into 4 classes.
(1) ultralow dielectric microwave dielectric ceramic, main representative is Al2O3-TiO2、Y2BaCuO5、MgAl2O4With
Mg2SiO4Deng, its εr≤ 20, quality factor q × f >=50000GHz, τƒ≤10 ppm/°C.It is mainly used in microwave base plate and height
End microwave device.
(2) low εrWith the microwave dielectric ceramic of high q-factor, mainly BaO-MgO-Ta2O5, BaO-ZnO-Ta2O5Or BaO-
MgO-Nb2O5,BaO-ZnO-Nb2O5System or the hybrid system MWDC material between them.Its εr=20～35, Q=(1～2) ×
104(under the GHz of f >=10), τƒ≈0.As medium in the microwave communication equipments such as the direct broadcasting satellite being mainly used in f >=8 GHz
Resonating device.
(3) medium εrWith the microwave dielectric ceramic of Q-value, it is mainly with BaTi4O9、Ba2Ti9O20(Zr, Sn) TiO4Etc. for
The MWDC material of base, its εr=35 ~ 45, Q=(6～9) × 103(under f=3～-4GHz), τƒ≤5 ppm/°C.It is mainly used in 4
～8 in microwave military radar in GHz frequency range and communication system as dielectric resonance device.
(4) high εrAnd the microwave dielectric ceramic that Q-value is relatively low, in being mainly used in 0.8～4GHz frequency range, civilian movement is led to
News system, this is also the emphasis of microwave dielectric ceramic research.Since the eighties, Kolar, Kato et al. in succession find and have studied
Perovskite-like tungsten bronze type BaO Ln2O3—TiO2Series (Ln=La, Sm, Nd or Pr etc. are called for short BLT system), composite perofskite
Structure C aO Li2O—Ln2O3—TiO2Series, lead base series material, Ca1-xLn2x/3TiO3It is contour εrMicrowave dielectric ceramic,
The wherein BaO Nd of BLT system2O3—TiO2Material dielectric constant reaches 90, lead base series (Pb, Ca) ZrO3Dielectric constant reaches
To 105.
The sintering temperature of the above material system is generally greater than 1300 ° of C, it is impossible to directly golden with the low melting point such as Ag and Cu
Belong to burning altogether and form multilayer ceramic capacitor.In recent years, along with LTCC Technology (Low Temperature Co-fired
Ceramics, LTCC) development and microwave multilayer device development requirement, research worker both domestic and external is to some low grade fever's systems
Material has carried out exploring widely and studying, and mainly uses devitrified glass or glassceramic composites system, because of low melting point
Glass has of a relatively high dielectric loss mutually, and the existence of glass phase substantially increases the dielectric loss of material.Therefore nothing is developed
The low fired microwave dielectric ceramic material of glass phase is the emphasis of current research.
Explore novel with exploitation can be during low fired microwave dielectric ceramic materials, the material bodies that intrinsic sintering temperature is low
System gets the attention and studies, but due to three performance indications (ε of microwave dielectric ceramicrWith Q f and τƒBetween)
It is that (see document: the restricting relation between microwave dielectric ceramic materials dielectric properties, Zhu Jianhua, Liang Fei, Wang is little for the mutual relation restricted
Red, Lv Wenzhong, electronic component and material, phase March the 3rd in 2005), meet three performance requirements and low temperature sintering be single-phase micro-
Ripple media ceramic is considerably less, mainly their temperature coefficient of resonance frequency is the most excessive or quality factor are on the low side and cannot be real
Border application requirement.Research major part to microwave-medium ceramics is the summary of experience drawn by great many of experiments at present, does not but have
There is complete theory to illustrate the relation of microstructure and dielectric properties, therefore, the most also cannot be from the composition of compound
With predict its microwave dielectric property such as temperature coefficient of resonance frequency and quality factor in structure, which greatly limits low
Temperature burning technology and the development of microwave multilayer device altogether.Explore and low-temperature sintering can have near-zero resonance frequency temperature with exploitation simultaneously
Coefficient (-10 ppm/DEG C≤τƒ≤+10 ppm/ DEG C) it is those skilled in the art with the microwave dielectric ceramic of higher figure of merit
Thirst for solving always but be difficult to the difficult problem succeeded all the time.
We are to consisting of LiBi2NbO6、LiLa2NbO6、LiNd2NbO6And LiBi2SbO6Series compound carried out micro-
The research of ripple dielectric properties, finds that their sintering temperature is less than 1200 DEG C, but only LiBi2NbO6There is near-zero resonance frequency
Temperature coefficient and high quality factor, LiBi2SbO6The temperature coefficient of resonance frequency τ of potteryƒ(respectively-91 ppm/ DEG C) bigger than normal and
And dielectric loss the highest and cannot as can be practical microwave-medium ceramics.LiLa2NbO6And LiNd2NbO6For quasiconductor
Resonance peak is not had at microwave frequency band.
Summary of the invention
It is an object of the invention to provide one can low-temperature sintering and to have good thermal stability normal with low-loss dielectric
Number microwave dielectric ceramic material and preparation method thereof.
The chemical composition of the microwave dielectric ceramic material of the present invention is LiBi2NbO6。
The preparation method step of this microwave dielectric ceramic material is:
(1) be 99.9%(percentage by weight by purity) more than Li2CO3、Bi2O3And Nb2O5Starting powder press
LiBi2NbO6Composition weigh dispensing.
(2) being mixed 12 hours by step (1) raw material wet ball-milling, ball-milling medium is dehydrated alcohol, big at 850 DEG C after drying
Pre-burning 6 hours in gas atmosphere.
(3), after adding binding agent pelletize in the powder that step (2) prepares, re-compacted molding, finally at 900 ~ 950 DEG C
Air atmosphere sinters 4 hours；Described binding agent uses mass concentration to be the poly-vinyl alcohol solution of 5%, the interpolation of polyvinyl alcohol
Amount accounts for the 3% of powder gross mass.
Advantages of the present invention: LiBi2NbO6Pottery sintering below 960 DEG C is good, and dielectric constant reaches 37.3～38.7,
The especially temperature coefficient τ of resonant frequencyƒLittle, temperature stability is good；Quality factor q f value is up to 64000-79000GHz, can be wide
The general manufacture for microwave devices such as various medium substrates, resonator and wave filter, can meet low temperature co-fired technology and microwave is many
The technology of layer device needs, and industrially has great using value.
Detailed description of the invention
Embodiment:
Table 1 shows 3 specific embodiments and the microwave dielectric property thereof of the different sintering temperatures constituting the present invention.Its system
Preparation Method as it has been described above, carry out the evaluation of microwave dielectric property by cylindrical dielectric resonator method.
This pottery can be widely used for the manufacture of the microwave devices such as various medium substrate, resonator and wave filter, can meet shifting
The technology of the systems such as dynamic communication and satellite communication needs.
Table 1:
Claims (1)
1. the composite oxides as the application of temperature-stable medium dielectric constant microwave medium microwave dielectric ceramic, it is characterised in that described
The chemical composition of composite oxides is: LiBi2NbO6；
The preparation method step of described composite oxides is:
(1) be 99.9%(percentage by weight by purity) more than Li2CO3、Bi2O3And Nb2O5Starting powder press LiBi2NbO6's
Composition weighs dispensing；
(2) being mixed 12 hours by step (1) raw material wet ball-milling, ball-milling medium is distilled water, 850 DEG C of air atmosphere after drying
Middle pre-burning 6 hours；
(3), after adding binding agent pelletize in the powder that step (2) prepares, re-compacted molding, finally at 900 ~ 950 DEG C of air
Atmosphere sinters 4 hours；Described binding agent uses mass concentration to be the poly-vinyl alcohol solution of 5%, and the addition of polyvinyl alcohol accounts for
The 3% of powder gross mass.
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| CN105198422A (en) * | 2015-10-08 | 2015-12-30 | 济南大学 | Li3Ni2NbO6 microwave dielectric material and preparation method thereof |
| CN105272212A (en) * | 2015-11-17 | 2016-01-27 | 桂林理工大学 | High-quality-factor temperature-stable middle-dielectric constant microwave dielectric ceramic Li3SmTi3O9 |
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| CN103539452A (en) * | 2013-10-22 | 2014-01-29 | 桂林理工大学 | Microwave dielectric ceramic Li2BiNb3O10 capable of being subjected to low-temperature sintering as well as preparation method thereof |
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