CN105198403A - Ultralow-dielectric-constant microwave dielectric ceramic Li3ZnBi5O11 and preparation method thereof - Google Patents
Ultralow-dielectric-constant microwave dielectric ceramic Li3ZnBi5O11 and preparation method thereof Download PDFInfo
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- CN105198403A CN105198403A CN201510637883.1A CN201510637883A CN105198403A CN 105198403 A CN105198403 A CN 105198403A CN 201510637883 A CN201510637883 A CN 201510637883A CN 105198403 A CN105198403 A CN 105198403A
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Abstract
The invention discloses ultralow-dielectric-constant microwave dielectric ceramic Li3ZnBi5O11 sinterable at low temperature, high in quality factor and temperature stable, and a preparation method thereof. The preparation method includes: 1, weighing and blending original powders of Li2CO3, ZnO and Bi2O3 higher than 99.9% in purity (weight by percent) according to the composition of Li3ZnBi5O11; 2, mixing raw material obtained in step 1 for 12 hours by wet ball-milling using distilled water as a ball-milling medium, and after drying, pre-sintering a mixture at 700 DEG C in air for 6 hours; 3, adding adhesive into powder obtained in step 2, performing compression forming after granulating, and performing sintering at 750-800 DEG C for 4 hours, wherein the adhesive is 5% polyvinyl alcohol solution, and the polyvinyl alcohol added is 3% of total weight of the powder. The prepared ceramic is well sinterable at 800 DEG C, has a dielectric constant reaching 12.3 to 13.1, a quality factor Qf up to 77000-95000 GHz and small temperature coefficient of resonance frequency and is highly worthy of industrial application.
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.
We are to composition Li
3zn
2bi
5o
11, Li
3zn
2la
5o
11, Li
3zn
2nd
5o
11, Li
3zn
2sm
5o
11serial monocline new compound carried out the research of microwave dielectric property, but only have Li
3zn
2bi
5o
11sintering temperature lower than 900 DEG C, and has near-zero resonance frequency temperature coefficient and high quality factor; Li
3zn
2la
5o
11and Li
3zn
2sm
5o
11temperature coefficient of resonance frequency is bigger than normal, and Li
3zn
2nd
5o
11pottery is too high and do not find resonance peak at microwave frequency band dielectric loss for semi-conductor, can not apply as microwave-medium ceramics.
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
3zn
2bi
5o
11.
Preparation method's step of this microwave dielectric ceramic material is:
(1) be 99.9%(weight percent by purity) more than Li
2cO
3, ZnO and Bi
2o
3starting powder press Li
3zn
2bi
5o
11composition 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
3zn
2bi
5o
11ceramic sintering temperature is low, and raw materials cost is low; Specific inductivity reaches 12.3 ~ 13.1, the temperature factor τ of its resonant frequency
?little, temperature stability is good; Quality factor q f value, up to 77000-95000GHz, 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 ultralow dielectric microwave dielectric ceramic for temperature-stable high quality factor, is characterized in that the chemical constitution of described microwave dielectric ceramic is: Li
3zn
2bi
5o
11;
Preparation method's concrete steps of described microwave dielectric ceramic are:
(1) be 99.9%(weight percent by purity) more than Li
2cO
3, ZnO and Bi
2o
3starting powder press Li
3zn
2bi
5o
11composition 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 |
---|---|---|---|---|
CN106187152A (en) * | 2016-07-20 | 2016-12-07 | 桂林理工大学 | Temperature-stable ultralow dielectric microwave dielectric ceramic Li2bi4ge3o13 |
CN106187133A (en) * | 2016-07-24 | 2016-12-07 | 桂林理工大学 | Temperature-stable ultralow dielectric microwave dielectric ceramic LiBi3si2o9 |
CN107311657A (en) * | 2017-07-11 | 2017-11-03 | 桂林理工大学 | Quaternary low-temperature sintered microwave dielectric ceramic material ZnO Li2O‑Bi2O3‑V2O5And preparation method thereof |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104261825A (en) * | 2014-09-19 | 2015-01-07 | 桂林理工大学 | Ultralow dielectric constant microwave dielectric ceramic Li3BiW8O27 capable of performing low-temperature sintering |
CN104311022A (en) * | 2014-10-16 | 2015-01-28 | 桂林理工大学 | Microwave dielectric ceramic Li2Bi3V7O23 with ultralow dielectric constant and preparation method thereof |
CN104311017A (en) * | 2014-10-12 | 2015-01-28 | 桂林理工大学 | Vanadium-based temperature-stable low-temperature sintering microwave dielectric ceramic and preparation method thereof |
-
2015
- 2015-10-07 CN CN201510637883.1A patent/CN105198403A/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104261825A (en) * | 2014-09-19 | 2015-01-07 | 桂林理工大学 | Ultralow dielectric constant microwave dielectric ceramic Li3BiW8O27 capable of performing low-temperature sintering |
CN104311017A (en) * | 2014-10-12 | 2015-01-28 | 桂林理工大学 | Vanadium-based temperature-stable low-temperature sintering microwave dielectric ceramic and preparation method thereof |
CN104311022A (en) * | 2014-10-16 | 2015-01-28 | 桂林理工大学 | Microwave dielectric ceramic Li2Bi3V7O23 with ultralow dielectric constant and preparation method thereof |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106187152A (en) * | 2016-07-20 | 2016-12-07 | 桂林理工大学 | Temperature-stable ultralow dielectric microwave dielectric ceramic Li2bi4ge3o13 |
CN106187133A (en) * | 2016-07-24 | 2016-12-07 | 桂林理工大学 | Temperature-stable ultralow dielectric microwave dielectric ceramic LiBi3si2o9 |
CN107311657A (en) * | 2017-07-11 | 2017-11-03 | 桂林理工大学 | Quaternary low-temperature sintered microwave dielectric ceramic material ZnO Li2O‑Bi2O3‑V2O5And preparation method thereof |
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Application publication date: 20151230 |