CN104557020B - A kind of sintered at ultra low temperature ultralow dielectric microwave dielectric ceramic and preparation method thereof - Google Patents
A kind of sintered at ultra low temperature ultralow dielectric microwave dielectric ceramic and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of sintered at ultra low temperature ultralow dielectric microwave dielectric ceramic LiBi2B3O8And preparation method thereof.(1) be 99.9%(percentage by weight by purity) more than Li2CO3、Bi2O3And H3BO3Starting powder press LiBi2B3O8Composition weigh dispensing；(2) by step (1) raw material wet ball-milling mix 12 hours, ball-milling medium is dehydrated alcohol, after drying in 520 DEG C of air atmosphere pre-burning 6 hours；(3) after adding binding agent pelletize in the powder that step (2) prepares, re-compacted molding, finally sinter 4 hours in 570 ~ 620 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 8.3～8.3, and its quality factor q f value is up to 112000 151000GHz, 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, television satellite accepter 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 DIELECTRIC CONSTANT 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 stability, 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.
The sintering temperature of the above material system is generally greater than 1300 ° of C, it is impossible to directly with low-cost Ag and Cu
Formation multilayer ceramic capacitor is burnt altogether at low-melting-point metal electrode.In recent years, along with LTCC Technology (Low
Temperature Co-fired Ceramics, LTCC) development and the requirement of microwave multilayer device development, both domestic and external grind
Study carefully personnel to have carried out exploring widely and studying to some low grade fever's system materials, mainly use devitrified glass or glass-ceramic
Composite system, has of a relatively high dielectric loss mutually because of low-melting glass, and the existence of glass phase substantially increases material
Dielectric loss.Therefore the emphasis that the low fired microwave dielectric ceramic material without glass phase is current research is developed.
Explore novel with exploitation can be during low fired microwave dielectric ceramic materials, the Li base that intrinsic sintering temperature is low
The material systems such as compound, Bi based compound, tungstates architecture compound and tellurate architecture compound get the attention with
Research, but due to three performance indications (ε of microwave dielectric ceramicrWith Q f and τfBetween) 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, electronics unit
Part and material, phase March the 3rd in 2005), satisfied three performance requirements and the single-phase microwave-medium ceramics of low temperature sintering are very
Few, their temperature coefficient of resonance frequency is the most excessive or quality factor are on the low side and cannot production application.At present to micro-
The research major part of ripple media ceramic is the summary of experience drawn by great many of experiments, does not but have complete theory micro-to illustrate
See the relation of structure and dielectric properties, the most also cannot predict its resonant frequency temperature from the composition of compound with structure
The microwave dielectric property such as coefficient and quality factor, explores and develops and low-temperature sintering can have again near-zero resonance frequency temperature coefficient
(-10 ppm/DEG C≤τƒ≤+10 ppm/ DEG C) with the microwave dielectric ceramic of higher figure of merit be those skilled in the art always
Thirst for solving but be difficult to the difficult problem succeeded all the time.
Summary of the invention
It is an object of the invention to provide one, to have good thermal stability dielectric ultralow with low-loss sintered at ultra low temperature normal
Number microwave dielectric ceramic material and preparation method thereof.
The chemical composition of the microwave dielectric ceramic material of the present invention is LiBi2B3O8。
The preparation method step of this microwave dielectric ceramic material is:
(1) be 99.9%(percentage by weight by purity) more than Li2CO3、Bi2O3And H3BO3Starting powder press
LiBi2B3O8Composition weigh dispensing.
(2) being mixed 12 hours by step (1) raw material wet ball-milling, ball-milling medium is dehydrated alcohol, big at 520 DEG C after drying
Pre-burning 6 hours in gas atmosphere.
(3), after adding binding agent pelletize in the powder that step (2) prepares, re-compacted molding, finally at 570 ~ 620 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: LiBi2B3O8Ceramic sintering temperature is less than 620 DEG C, and dielectric constant reaches 8.3～8.8, and it is humorous
The temperature coefficient τ of vibration frequencyƒLittle, temperature stability is good；Quality factor q f value is up to 112000-151000GHz, can be widely used for
The manufacture of the microwave devices such as various medium substrates, resonator and wave filter, can meet low temperature co-fired technology and microwave multilayer device
Technology need, industrially have great using value.
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 sintered at ultra low temperature ultralow dielectric microwave dielectric ceramic, it is characterised in that the chemistry of described microwave dielectric ceramic
Consist of: LiBi2B3O8；
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、Bi2O3And H3BO3Starting powder press LiBi2B3O8's
Composition weighs dispensing；
(2) being mixed 12 hours by step (1) raw material wet ball-milling, ball-milling medium is dehydrated alcohol, at 520 DEG C of air gas after drying
Pre-burning 6 hours in atmosphere；
(3), after adding binding agent pelletize in the powder that step (2) prepares, re-compacted molding, finally at 570 ~ 620 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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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103011810A (en) * | 2012-12-07 | 2013-04-03 | 桂林理工大学 | Low-temperature sinterable lithium-containing garnet structure microwave dielectric ceramic Li2Ca2BiV3O12 and its preparation method |
| CN103539452A (en) * | 2013-10-22 | 2014-01-29 | 桂林理工大学 | Microwave dielectric ceramic Li2BiNb3O10 capable of being subjected to low-temperature sintering as well as preparation method thereof |
| 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 |
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2014
- 2014-12-27 CN CN201410825333.8A patent/CN104557020B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103011810A (en) * | 2012-12-07 | 2013-04-03 | 桂林理工大学 | Low-temperature sinterable lithium-containing garnet structure microwave dielectric ceramic Li2Ca2BiV3O12 and its preparation method |
| CN103539452A (en) * | 2013-10-22 | 2014-01-29 | 桂林理工大学 | Microwave dielectric ceramic Li2BiNb3O10 capable of being subjected to low-temperature sintering as well as preparation method thereof |
| 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 |
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