CN104446377B - Temperature-stable microwave dielectric ceramic LiZn2b3o7and preparation method thereof - Google Patents
Temperature-stable microwave dielectric ceramic LiZn2b3o7and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of temperature-stable ultralow dielectric microwave dielectric ceramic LiZn2B3O7And preparation method thereof.(1) be 99.9%(percentage by weight by purity) more than Li2CO3, ZnO and H3BO3Starting powder press LiZn2B3O7Composition weigh dispensing；(2) by step (1) raw material wet ball-milling mix 12 hours, ball-milling medium is absolute ethyl alcohol, after drying in 800 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 850 ~ 890 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.Ceramic post sintering prepared by the present invention is good, and dielectric constant reaches 5.5～5.9, and its quality factor q f value is up to 121000 147000GHz, 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 substrate, the resonance that microwave frequency uses
Dielectric ceramic materials of microwave device such as device and wave filter 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.
Three performance indications (ε due to 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, electronic component
With material, phase March the 3rd in 2005), the single-phase microwave-medium ceramics meeting three performance requirements is considerably less, is mainly theirs
Temperature coefficient of resonance frequency is the most excessive or quality factor are on the low side and cannot application request.At present to microwave-medium ceramics
Research major part be the summary of experience drawn by great many of experiments, but there is no complete theory to illustrate microstructure and Jie
The relation of electrical property, therefore, the most also cannot predict its temperature coefficient of resonance frequency from the composition of compound with structure
With the microwave dielectric properties such as quality factor, explore and develop near-zero resonance frequency temperature coefficient (-10 ppm/DEG C≤τƒ≤+10
Ppm/ DEG C) it is that those skilled in the art thirst for solving always with the serial differing dielectric constant microwave dielectric ceramic of higher figure of merit
Determine but be difficult to the difficult problem succeeded all the time, which greatly limits the development of microwave dielectric ceramic and device.We
To composition LiZn2B3O7、LiMg2B3O7、LiCu2B3O7、LiNi2B3O7Series compound carried out grinding of microwave dielectric property
Study carefully, find that their sintering temperature is less than 900 DEG C, the most only LiZn2B3O7There are near-zero resonance frequency temperature coefficient and high-quality
Factor.LiMg2B3O7The temperature coefficient of resonance frequency τ of potteryƒ(respectively+17 ppm/ DEG C) bigger than normal and cannot be as practical
Microwave-medium ceramics;And LiCu2B3O7、LiNi2B3O7For semiconductor, its dielectric loss is too big and cannot make pottery as microwave-medium
Porcelain.
Summary of the invention
It is an object of the invention to provide one and there is good thermal stability and low-loss ultralow dielectric micro-wave dielectric
Ceramic material and preparation method thereof.
The chemical composition of the microwave dielectric ceramic material of the present invention is LiZn2B3O7。
The preparation method step of this microwave dielectric ceramic material is:
(1) be 99.9%(percentage by weight by purity) more than Li2CO3, ZnO and H3BO3Starting powder press
LiZn2B3O7Composition weigh dispensing.
(2) being mixed 12 hours by step (1) raw material wet ball-milling, ball-milling medium is absolute ethyl alcohol, big at 800 DEG C after drying
Pre-burning 6 hours in gas atmosphere.
(3), after adding binding agent granulation in the powder that step (2) prepares, re-compacted shaping, finally at 850 ~ 890 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: LiZn2B3O7Ceramic dielectric constant reaches 5.5～5.9, the temperature coefficient τ of its resonant frequencyƒ
Little, temperature stability is good；Quality factor q f value is up to 121000-147000GHz, can be widely used for various dielectric resonator and filter
The manufacture of the microwave devices such as ripple device, can meet the technology needs of low temperature co-fired technology and microwave multilayer device, industrially have
Using value greatly.
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 medium substrate, resonator and wave filter, can meet shifting
The technology of the systems such as dynamic communication and satellite communication needs.
Table 1:
Claims (1)
1. a temperature-stable ultralow dielectric microwave dielectric ceramic, it is characterised in that the chemistry of described microwave dielectric ceramic
Consist of: LiZn2B3O7；
The preparation method of described microwave dielectric ceramic concretely comprises the following steps:
(1) be 99.9%(percentage by weight by purity) more than Li2CO3, ZnO and H3BO3Starting powder press LiZn2B3O7Group
Become to weigh dispensing；
(2) being mixed 12 hours by step (1) raw material wet ball-milling, ball-milling medium is absolute ethyl alcohol, at 800 DEG C of air gas 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 850 ~ 890 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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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105439554A (en) * | 2015-12-19 | 2016-03-30 | 桂林理工大学 | Temperature-stable microwave dielectric ceramic Li4Zn3B4O11 with low dielectric constant and preparation method thereof |
| CN105523758A (en) * | 2016-02-20 | 2016-04-27 | 桂林理工大学 | Temperature-stable microwave dielectric ceramic SrZn3B4O10 with ultralow dielectric constant as well as preparation method of microwave dielectric ceramic SrZn3B4O10 |
| CN105523757A (en) * | 2016-02-20 | 2016-04-27 | 桂林理工大学 | Temperature-stable microwave dielectric ceramic Li3Zn2B3O8 capable of realizing low-temperature sintering and preparation method of microwave dielectric ceramic Li3Zn2B3O8 |
| CN105645950A (en) * | 2016-02-20 | 2016-06-08 | 桂林理工大学 | Microwave dielectric ceramic Li3ZnB3O7 with ultralow dielectric constant and preparation method of microwave dielectric ceramic Li3ZnB3O7 |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103880422A (en) * | 2014-04-06 | 2014-06-25 | 桂林理工大学 | Microwave dielectric ceramic Li3Nb3B2O12 sintered at ultralow temperature and preparation method thereof |
| CN104003723A (en) * | 2014-05-24 | 2014-08-27 | 桂林理工大学 | Microwave dielectric ceramic Li3Zn4NbO8 capable of realizing low-temperature sintering and preparation method thereof |
| CN104003720A (en) * | 2014-05-17 | 2014-08-27 | 桂林理工大学 | Microwave dielectric ceramic Li2Zn2W2O9 capable of being sintered at low temperature and preparation method thereof |
| CN104045344A (en) * | 2014-06-02 | 2014-09-17 | 桂林理工大学 | Low temperature sinterable microwave dielectric ceramic Li2Zn3WO7 and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103880422A (en) * | 2014-04-06 | 2014-06-25 | 桂林理工大学 | Microwave dielectric ceramic Li3Nb3B2O12 sintered at ultralow temperature and preparation method thereof |
| CN104003720A (en) * | 2014-05-17 | 2014-08-27 | 桂林理工大学 | Microwave dielectric ceramic Li2Zn2W2O9 capable of being sintered at low temperature and preparation method thereof |
| CN104003723A (en) * | 2014-05-24 | 2014-08-27 | 桂林理工大学 | Microwave dielectric ceramic Li3Zn4NbO8 capable of realizing low-temperature sintering and preparation method thereof |
| CN104045344A (en) * | 2014-06-02 | 2014-09-17 | 桂林理工大学 | Low temperature sinterable microwave dielectric ceramic Li2Zn3WO7 and preparation method thereof |
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Effective date of registration: 20180828 Address after: 536000 the Guangxi Zhuang Autonomous Region Beihai Haicheng District Guangxi Beihai Industrial Park New Future Science Park Patentee after: Guangxi New Future Information Industry Co., Ltd. Address before: No. 12, Jian Gong Road, Guilin, the Guangxi Zhuang Autonomous Region Patentee before: Guilin University of Technology |