CN104311022A - Microwave dielectric ceramic Li2Bi3V7O23 with ultralow dielectric constant and preparation method thereof - Google Patents
Microwave dielectric ceramic Li2Bi3V7O23 with ultralow dielectric constant and preparation method thereof Download PDFInfo
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- CN104311022A CN104311022A CN201410548164.8A CN201410548164A CN104311022A CN 104311022 A CN104311022 A CN 104311022A CN 201410548164 A CN201410548164 A CN 201410548164A CN 104311022 A CN104311022 A CN 104311022A
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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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Abstract
The invention discloses microwave dielectric ceramic Li2Bi3V7O23 with an ultralow dielectric constant and a preparation method thereof. The ceramic can be sintered at low temperature and has stable temperature. The preparation method comprises the steps of (1) weighing original powders of Li2CO3, Bi2O3 and V2O5 with the purity over 99.9% (by weight percent) according to the components of the Li2Bi3V7O23; (2) ball milling and mixing the raw materials of the step (1) for 12 hours by a wet method, drying and then presintering for 6 hours in 700DEG C atmosphere environment, wherein the ball milling medium is distilled water; and (3) adding a binder into the powder prepared in the step (2) and then prilling, pressing and molding, and finally sintering for 4 hours in 750-800DEG C atmosphere environment, wherein the binder is polyvinyl alcohol solution with the mass concentration 5%, and the amount of the polyvinyl alcohol is 3% of total mass of the powder. The ceramic prepared by the method can be sintered at 750-800DEG C, the dielectric constant reaches 15.2-16.4, the quality factor Qf reaches 71000-92000GHz, the temperature coefficient of resonance frequency is small, and the ceramic has great application value in industry.
Description
Technical field
The present invention relates to dielectric ceramic material, particularly relate to dielectric ceramic material of the microwave devices such as ceramic substrate, resonator and the 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>=3000 GHz; (3) the temperature factor τ of resonant frequency
?little of as far as possible to ensure the thermostability that device has had, general requirement-10 ppm/DEG C≤τ
?≤+10 ppm/ 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
?≤ 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 composite system MWDC material between them.Its ε
r=20 ~ 35, 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 ~ 45, Q=(6 ~ 9) × 10
3(under f=3 ~-4GHz), τ
?≤ 5 ppm/ ° C.Be mainly used in microwave military radar in 4 ~ 8 GHz 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 (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 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 meet application request.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 with exploitation can low-temperature sintering have simultaneously near-zero resonance frequency temperature coefficient (-10 ppm/DEG C≤τ
?≤+10 ppm/ 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.
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 ultralow dielectric microwave dielectric ceramic material and preparation method thereof.
The chemical constitution of microwave dielectric ceramic material of the present invention is Li
2bi
3v
7o
23.
Preparation method's step of this microwave dielectric ceramic material is:
(1) be 99.9%(weight percent by purity) more than Li
2cO
3, Bi
2o
3and V
2o
5starting powder press Li
2bi
3v
7o
23composition 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 700 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 750 ~ 800 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: Li
2bi
3v
7o
23ceramic sintering temperature is low, and raw materials cost is low; Specific inductivity reaches 15.2 ~ 16.4, the temperature factor τ of its resonant frequency
?little, temperature stability is good; Quality factor q f value, up to 71000-92000GHz, can be widely used in the manufacture of the microwave devices such as various medium substrate, 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 medium substrate, 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 ultralow dielectric microwave dielectric ceramic, is characterized in that the chemical constitution of described microwave dielectric ceramic is: Li
2bi
3v
7o
23;
Preparation method's concrete steps of described microwave dielectric ceramic are:
(1) be 99.9%(weight percent by purity) more than Li
2cO
3, Bi
2o
3and V
2o
5starting powder press Li
2bi
3v
7o
23composition 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 700 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 750 ~ 800 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.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104817324A (en) * | 2015-04-27 | 2015-08-05 | 桂林理工大学 | Temperature-stable microwave dielectric ceramics Li<2>LaVO<5> with low dielectric constants |
CN105174938A (en) * | 2015-10-09 | 2015-12-23 | 桂林理工大学 | Resistance material Li4Bi3Nb3O14 with high curie-point positive temperature coefficient and preparation method of resistance material |
CN105198403A (en) * | 2015-10-07 | 2015-12-30 | 桂林理工大学 | Ultralow-dielectric-constant microwave dielectric ceramic Li3ZnBi5O11 and preparation method thereof |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2003083969A1 (en) * | 2002-03-28 | 2003-10-09 | Mitsubishi Chemical Corporation | Positive electrode material for lithium secondary cell and secondary cell using the same, and method for producing positive electrode material for lithium secondary cell |
CN103922723A (en) * | 2014-04-06 | 2014-07-16 | 桂林理工大学 | Ultralow temperature sintered microwave dielectric ceramic Li3V3Bi2O12 and preparation method thereof |
-
2014
- 2014-10-16 CN CN201410548164.8A patent/CN104311022B/en not_active Expired - Fee Related
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2003083969A1 (en) * | 2002-03-28 | 2003-10-09 | Mitsubishi Chemical Corporation | Positive electrode material for lithium secondary cell and secondary cell using the same, and method for producing positive electrode material for lithium secondary cell |
CN103922723A (en) * | 2014-04-06 | 2014-07-16 | 桂林理工大学 | Ultralow temperature sintered microwave dielectric ceramic Li3V3Bi2O12 and preparation method thereof |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104817324A (en) * | 2015-04-27 | 2015-08-05 | 桂林理工大学 | Temperature-stable microwave dielectric ceramics Li<2>LaVO<5> with low dielectric constants |
CN105198403A (en) * | 2015-10-07 | 2015-12-30 | 桂林理工大学 | Ultralow-dielectric-constant microwave dielectric ceramic Li3ZnBi5O11 and preparation method thereof |
CN105174938A (en) * | 2015-10-09 | 2015-12-23 | 桂林理工大学 | Resistance material Li4Bi3Nb3O14 with high curie-point positive temperature coefficient and preparation method of resistance material |
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