CN104311021B - A kind of ultralow dielectric microwave dielectric ceramic and preparation method thereof - Google Patents
A kind of ultralow dielectric microwave dielectric ceramic and preparation method thereof Download PDFInfo
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- CN104311021B CN104311021B CN201410537383.6A CN201410537383A CN104311021B CN 104311021 B CN104311021 B CN 104311021B CN 201410537383 A CN201410537383 A CN 201410537383A CN 104311021 B CN104311021 B CN 104311021B
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Abstract
The invention discloses a kind of low temperature sintering ultralow dielectric microwave dielectric ceramic Ca5V3O12F and preparation method thereof.(1) be 99.9%(percentage by weight by purity) more than CaF2、CaCO3And V2O5Starting powder press Ca5V3O12The composition of F weighs dispensing；(2) by step (1) raw material wet ball-milling mix 12 hours, ball-milling medium is distilled water, after drying in 850 DEG C of air atmosphere pre-burning 6 hours；(3) after adding binding agent granulation in the powder that step (2) prepares, re-compacted shaping, finally sinter 4 hours in 900 ~ 930 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.Pottery prepared by the present invention is good at 900 ~ 930 DEG C of sintering, and dielectric constant reaches 9.7～10.4, and its quality factor q f value is up to 66400-72100GHz, 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 resonator and the filter that microwave frequency uses
Dielectric ceramic materials of microwave device such as ripple device 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, telstar recipient 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 permittivity 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 endurance, 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, researcher both domestic and external is to some low 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 Li base that intrinsic sintering temperature is low
The material systems such as compound, Bi based compound, tungstates architecture compound and tellurate architecture compound get the attention with
Research, but due to three performance indications (ε of microwave dielectric ceramicrWith Q f and τƒBetween) be mutually restriction relation (see
Document: the restricting relation between microwave dielectric ceramic materials dielectric properties, Zhu Jianhua, Liang Fei, Wang little Hong, Lv Wenzhong, electronics unit
Part and material, phase March the 3rd in 2005), satisfied three performance requirements and the single-phase microwave-medium ceramics of low temperature sintering are very
Few, mainly their temperature coefficient of resonance frequency is the most excessive or quality factor are on the low side and cannot application request.Mesh
The front research major part to microwave-medium ceramics is the summary of experience drawn by great many of experiments, does not but have complete theory
Illustrate the relation of microstructure and dielectric properties, therefore, the most also cannot predict it from the composition of compound with structure
The microwave dielectric property such as temperature coefficient of resonance frequency and quality factor, which greatly limits low temperature co-fired technology and micro-
The development of ripple multilayer device.Explore and low-temperature sintering can have near-zero resonance frequency temperature coefficient and higher quality with exploitation simultaneously
The ultralow dielectric microwave dielectric ceramic of factor be those skilled in the art always thirst for solve but be difficult to all the time succeed
A difficult problem.
We are to composition Ba5V3O12F、Ca5V3O12F、Sr5V3O12F and Mg5V3O12The series compound of F has carried out micro-
The research of ripple dielectric properties, finds that their sintering temperature is below 960 DEG C, Ca5V3O12F、Ba5V3O12F and Mg5V3O12F dielectric
Constant only has 7 to 11, belongs to ultralow dielectric microwave dielectric ceramic, but only Ca5V3O12F has near-zero resonance frequency temperature
Coefficient and high quality factor, Ba5V3O12F and Mg5V3O12Temperature coefficient of resonance frequency (the τ respectively-76 bigger than normal of F pottery
Ppm/ DEG C and-42 ppm/ DEG C).Sr5V3O12The dielectric loss of F too greatly cannot be as microwave dielectric ceramic.
Summary of the invention
It is an object of the invention to provide and a kind of have good heat endurance and low-loss, low temperature sintering is ultralow simultaneously
Dielectric constant microwave dielectric ceramic material and preparation method thereof.
The chemical composition of the microwave dielectric ceramic material of the present invention is Ca5V3O12F。
The preparation method step of this microwave dielectric ceramic material is:
(1) be 99.9%(percentage by weight by purity) more than CaF2、CaCO3And V2O5Starting powder press Ca5V3O12F
Composition weigh dispensing.
(2) being mixed 12 hours by step (1) raw material wet ball-milling, ball-milling medium is distilled water, at 850 DEG C of air after drying
Pre-burning 6 hours in atmosphere.
(3), after adding binding agent granulation in the powder that step (2) prepares, re-compacted shaping, finally at 900 ~ 930 DEG C
Air atmosphere sinters 4 hours；Described binding agent uses mass concentration to be the poly-vinyl alcohol solution of 5%, polyvinyl alcohol addition
Account for the 3% of powder gross mass.
Advantages of the present invention: Ca5V3O12F ceramic sintering temperature is low, and cost of material is low；Dielectric constant reaches 9.7～10.4,
The temperature coefficient τ of its resonant frequencyƒLittle, temperature stability is good；Quality factor q f value is up to 66400-72100GHz, can extensively use
In the manufacture of the microwave devices such as various dielectric resonators and wave filter, low temperature co-fired technology and the skill of microwave multilayer device can be met
Art 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 dielectric resonator and wave filter, can meet mobile communication
Need with the technology of the system such as satellite communication.
Table 1:
Claims (1)
1. possessing a ultralow dielectric microwave dielectric ceramic for near-zero resonance frequency temperature coefficient and high quality factor, it is special
Levy and be that the chemical composition of described microwave dielectric ceramic is: Ca5V3O12F；
The preparation method of described microwave dielectric ceramic concretely comprises the following steps:
(1) be 99.9%(percentage by weight by purity) more than CaF2、CaCO3And V2O5Starting powder press Ca5V3O12The group of F
Become to weigh 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 granulation in the powder that step (2) prepares, re-compacted shaping, finally at 900 ~ 930 DEG C of air
Atmosphere sinters 4 hours；Described binding agent uses mass concentration to be the poly-vinyl alcohol solution of 5%, and polyvinyl alcohol addition accounts for powder
The 3% of end gross mass.
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| CN201410537383.6A CN104311021B (en) | 2014-10-13 | 2014-10-13 | A kind of ultralow dielectric microwave dielectric ceramic and preparation method thereof |
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| CN102875148B (en) * | 2012-10-17 | 2013-12-18 | 桂林理工大学 | Microwave dielectric ceramic LiCa3(Mg1-xZnx)V3O12 capable of being sintered at low temperature and preparation method |
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