CN104725044A - Temperature-stable microwave dielectric ceramic LiMg2V7O20 with ultra-low dielectric constant - Google Patents
Temperature-stable microwave dielectric ceramic LiMg2V7O20 with ultra-low dielectric constant Download PDFInfo
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- CN104725044A CN104725044A CN201510099849.3A CN201510099849A CN104725044A CN 104725044 A CN104725044 A CN 104725044A CN 201510099849 A CN201510099849 A CN 201510099849A CN 104725044 A CN104725044 A CN 104725044A
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Abstract
The invention discloses temperature-stable microwave dielectric ceramic LiMg2V7O20 with an ultra-low dielectric constant and a preparation method of the ceramic LiMg2V7O20. The preparation method comprises the following steps: (1) weighing and proportioning Li2CO3, MgO and V2O5 original powder which have purities of 99.9wt% or above; (2) carrying out wet ball-milling mixing on the raw material obtained in the step (1) for 12h, drying and then presintering in a 750 DEG C air atmosphere for 6h, wherein the ball milling medium is distilled water; and (3) adding a binder to the powder obtained in the step (2), granulating, carrying out compression moulding, and finally sintering for 4h in a 800-850 DEG C air atmosphere, wherein the binder is a polyvinyl alcohol solution with a mass concentration of 5% and the addition amount of polyvinyl alcohol accounts for 3% of the total mass of the powder. The prepared ceramic has good sintering performance at a temperature of 850 DEG C or below; the dielectric constant reaches 16.4-17.3, the quality factor (QF) value is high up to 97000-143000GHz, and the temperature coefficient of resonance frequency is small, and thus the temperature-stable microwave dielectric ceramic LiMg2V7O20 with an ultra-low dielectric constant has extremely large industrial application value.
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, resonator is widely used as in modern communication, wave filter, the components and parts such as dielectric substrate and medium wave circuit, it is the key foundation material of modern communication technology, at portable mobile phone, automobile telephone, cordless telephone, there is very important application the aspects such as telestar susceptor and military radar, in the miniaturization of modern communication instrument, increasing effect is just being played in integrated process.
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>=3000GHz; (3) the temperature factor τ of resonant frequency
flittle of as far as possible to ensure the thermostability that device has had, general requirement-10ppm/ DEG C≤τ
f≤+10ppm/ 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
ftoo 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
f≤ 10ppm/ DEG 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 f>=10GHz), τ
f≈ 0.Be mainly used in the microwave communication equipments such as the direct broadcasting satellite of f >=8GHz 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
f≤ 5ppm/ DEG C.Be mainly used in microwave military radar in 4 ~ 8GHz 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 DEG 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 (LowTemperature 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
f) 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 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 and low-temperature sintering can have near-zero resonance frequency temperature coefficient (-10ppm/ DEG C≤τ with exploitation simultaneously
f≤+10ppm/ 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.
We are to composition LiMg
2v
7o
20, LiCu
2v
7o
20, LiNi
2v
7o
20series compound carried out the research of microwave dielectric property, find that their sintering temperature is lower than 900 DEG C, but only have LiMg
2v
7o
20there is near-zero resonance frequency temperature coefficient and high quality factor, LiNi
2v
7o
20the temperature coefficient of resonance frequency τ of pottery
f(being respectively-91ppm/ DEG C) bigger than normal and dielectric loss is also higher and cannot as microwave-medium ceramics that can be practical.LiCu
2v
7o
20for ionophore does not have resonance peak at microwave frequency band.
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 LiMg
2v
7o
20.
Preparation method's step of this microwave dielectric ceramic material is:
(1) by purity be the Li of more than 99.9% (weight percent)
2cO
3, MgO and V
2o
5starting powder press LiMg
2v
7o
20composition 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 750 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 800 ~ 850 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: LiMg
2v
7o
20ceramic sintering temperature is low, and raw materials cost is low; Specific inductivity reaches 16.4 ~ 17.3, the temperature factor τ of its resonant frequency
flittle, temperature stability is good; Quality factor q f value, up to 97000-143000GHz, 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.
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 temperature-stable ultralow dielectric microwave dielectric ceramic, is characterized in that the chemical constitution of described microwave dielectric ceramic is: LiMg
2v
7o
20;
Preparation method's concrete steps of described microwave dielectric ceramic are:
(1) be 99.9%(weight percent by purity) more than Li
2cO
3, MgO and V
2o
5starting powder press LiMg
2v
7o
20composition 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 750 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 800 ~ 850 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 |
---|---|---|---|---|
CN105801118A (en) * | 2016-03-03 | 2016-07-27 | 三峡大学 | Low-loss temperature-stable type low dielectric constant microwave dielectric ceramic LiMg2Nb7O20 |
CN105859284A (en) * | 2016-04-01 | 2016-08-17 | 桂林理工大学 | Low-loss and low-dielectric-constant microwave dielectric ceramic Li3MgNbO5 |
CN107867859A (en) * | 2016-09-22 | 2018-04-03 | 施海月 | Li0.8Mg4.1V3O12The preparation method of microwave-medium ceramics |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104058748A (en) * | 2014-06-30 | 2014-09-24 | 桂林理工大学 | Microwave dielectric ceramic LiMg2V3O10 allowing low-temperature sintering and preparation method thereof |
-
2015
- 2015-03-06 CN CN201510099849.3A patent/CN104725044A/en active Pending
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104058748A (en) * | 2014-06-30 | 2014-09-24 | 桂林理工大学 | Microwave dielectric ceramic LiMg2V3O10 allowing low-temperature sintering and preparation method thereof |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105801118A (en) * | 2016-03-03 | 2016-07-27 | 三峡大学 | Low-loss temperature-stable type low dielectric constant microwave dielectric ceramic LiMg2Nb7O20 |
CN105859284A (en) * | 2016-04-01 | 2016-08-17 | 桂林理工大学 | Low-loss and low-dielectric-constant microwave dielectric ceramic Li3MgNbO5 |
CN107867859A (en) * | 2016-09-22 | 2018-04-03 | 施海月 | Li0.8Mg4.1V3O12The preparation method of microwave-medium ceramics |
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