CN105330261A - Temperature-stable microwave dielectric ceramic Li2MgGeO4 with high quality factor and preparation method thereof - Google Patents
Temperature-stable microwave dielectric ceramic Li2MgGeO4 with high quality factor and preparation method thereof Download PDFInfo
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Abstract
The invention discloses application of composite oxide as temperature-stable ultra-low dielectric constant microwave dielectric ceramic with a high quality factor. The application is realized by the following steps of firstly, weighing and blending raw powder of Li2CO3, MgO and GeO2 with the purity of 99.9 percent or over 99.9 percent (weight percentage) according to the composition of Li2MgGeO4; secondly, performing wet ball mill mixing on raw materials in the first step for 12 hours, wherein a ball milling medium is distilled water, drying and then presintering in the atmosphere of 850DEG C for 6 hours; thirdly, adding a binder in powder obtained in the second step, granulating, performing compression molding, and finally sintering in the atmosphere of 900 to 950DEG C for 4 hours, wherein the binder adopts polyvinyl alcohol solution with mass concentration of 5 percent, and the addition amount of polyvinyl alcohol accounts for 3 percent of total mass of the powder. The ceramic prepared by the invention is good in sintering property at the temperature below 950DEG C; a dielectric constant of the ceramic reaches 15.4 to 16.3, a quality factor Qf value of the ceramic is as high as 99,000 to 163,000GHz, and a temperature coefficient of resonance frequency is small; the temperature-stable ultra-low dielectric constant microwave dielectric 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>=3000GHz; (3) the temperature factor τ of resonant frequency
?little of as far as possible to ensure the thermostability that device has had, general requirement-10ppm/ DEG C≤τ
?≤+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
?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
?≤ 10ppm/ ° of 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
?≈ 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
?≤ 5ppm/ ° of 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 ° 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 (LowTemperatureCo-firedCeramics, 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 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
?≤+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.
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
2mgGeO
4.
Preparation method's step of this microwave dielectric ceramic material is:
(1) be 99.9%(weight percent by purity) more than Li
2cO
3, MgO and GeO
2starting powder press Li
2mgGeO
4composition 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 850 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 900 ~ 950 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
2mgGeO
4ceramic sintering temperature is low, and raw materials cost is low; Its quality factor q f value is up to 99000-165000GHz, and specific inductivity reaches 15.4 ~ 16.3, the temperature factor τ of its resonant frequency
?little, temperature stability is good; The manufacture of the microwave devices such as various substrate, dielectric resonator and wave filter can be widely used in, the technology needs of low temperature co-fired technology and microwave multilayer device can be met.
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. composite oxides are as an application for temperature-stable high quality factor microwave dielectric ceramic, it is characterized in that the chemical constitution of described microwave dielectric ceramic is: Li
2mgGeO
4;
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 GeO
2starting powder press Li
2mgGeO
4composition 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 850 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 900 ~ 950 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 (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105777078A (en) * | 2016-05-23 | 2016-07-20 | 桂林理工大学 | Low-loss temperature-stable type ultralow dielectric constant microwave dielectric ceramic Mg3Y2Ge3O12 |
CN106187105A (en) * | 2016-07-19 | 2016-12-07 | 桂林理工大学 | High quality factor temperature-stable dielectric constant microwave dielectric ceramic Li2baMgGeO5 |
CN106187102A (en) * | 2016-07-19 | 2016-12-07 | 桂林理工大学 | High quality factor temperature-stable microwave dielectric ceramic Li2mgGe2o6 |
CN106278241A (en) * | 2016-07-19 | 2017-01-04 | 桂林理工大学 | High quality factor temperature-stable dielectric constant microwave dielectric ceramic Li2srSnO4 |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104628369A (en) * | 2015-02-05 | 2015-05-20 | 桂林理工大学 | Temperature-stable microwave dielectric ceramic Li2Mg4Si4O13 with ultra-low dielectric constant |
CN104909748A (en) * | 2015-05-23 | 2015-09-16 | 桂林理工大学 | Temperature stable low dielectric constant microwave dielectric ceramic BaLi2Mg2V8O24 |
-
2015
- 2015-11-30 CN CN201510845545.7A patent/CN105330261A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104628369A (en) * | 2015-02-05 | 2015-05-20 | 桂林理工大学 | Temperature-stable microwave dielectric ceramic Li2Mg4Si4O13 with ultra-low dielectric constant |
CN104909748A (en) * | 2015-05-23 | 2015-09-16 | 桂林理工大学 | Temperature stable low dielectric constant microwave dielectric ceramic BaLi2Mg2V8O24 |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105777078A (en) * | 2016-05-23 | 2016-07-20 | 桂林理工大学 | Low-loss temperature-stable type ultralow dielectric constant microwave dielectric ceramic Mg3Y2Ge3O12 |
CN106187105A (en) * | 2016-07-19 | 2016-12-07 | 桂林理工大学 | High quality factor temperature-stable dielectric constant microwave dielectric ceramic Li2baMgGeO5 |
CN106187102A (en) * | 2016-07-19 | 2016-12-07 | 桂林理工大学 | High quality factor temperature-stable microwave dielectric ceramic Li2mgGe2o6 |
CN106278241A (en) * | 2016-07-19 | 2017-01-04 | 桂林理工大学 | High quality factor temperature-stable dielectric constant microwave dielectric ceramic Li2srSnO4 |
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