CN104446433B - Temperature-stable ultralow dielectric microwave dielectric ceramic Li3al2p3o12 - Google Patents
Temperature-stable ultralow dielectric microwave dielectric ceramic Li3al2p3o12 Download PDFInfo
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- CN104446433B CN104446433B CN201410634371.5A CN201410634371A CN104446433B CN 104446433 B CN104446433 B CN 104446433B CN 201410634371 A CN201410634371 A CN 201410634371A CN 104446433 B CN104446433 B CN 104446433B
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Abstract
The invention discloses a kind of low temperature sintering temperature-stable ultralow dielectric microwave dielectric ceramic Li3Al2P3O12And preparation method thereof.(1) be 99.9%(percentage by weight by purity) more than Li2CO3、Al2O3And NH4H2PO4Starting powder press Li3Al2P3O12Composition 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 ~ 900 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.Pottery prepared by the present invention is good at 850 ~ 900 DEG C of sintering, and dielectric constant reaches 6.2～6.7, and its quality factor q f value is up to 81000-122000GHz, 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 dielectric loss tan δ make an uproar to reduce
Sound, typically requires Qf >=3000 GHz;(3) the temperature coefficient τ of resonant frequencyƒThe least to ensure the heat that device has had
Stability, general requirement-10 ppm/DEG C≤τƒ≤+10 ppm/℃.Just have tried to from late 1930s in the world by
Dielectric substance is applied to microwave technology, and prepares TiO2Microwave dielectric filter, but its temperature coefficient of resonance frequency τƒToo
Greatly cannot be practical.Since the seventies in last century, start the large-scale development to medium ceramic material, according to
Relative dielectric constant εrSize different from use frequency range, generally can have been developed that and the microwave-medium ceramics developed
It 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 golden with the low melting point such as Ag and Cu
Belong to burning altogether and form multilayer ceramic capacitor.In recent years, along with LTCC Technology (Low Temperature Co-fired
Ceramics, LTCC) development and microwave multilayer device development requirement, researcher both domestic and external is to some low fever's systems
Material has carried out exploring widely and studying, and mainly uses devitrified glass or glassceramic composites system, because of low melting point
Glass has of a relatively high dielectric loss mutually, and the existence of glass phase substantially increases the dielectric loss of material.Therefore nothing is developed
The low fired microwave dielectric ceramic material of glass phase is the emphasis of current research.
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 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), meet three performance requirements and the single-phase microwave-medium ceramics of low temperature sintering is considerably less,
Mainly their temperature coefficient of resonance frequency is the most excessive or quality factor are on the low side and cannot application request.The most right
The research major part of microwave-medium ceramics is the summary of experience drawn by great many of experiments, does not but have complete theory to illustrate
Microstructure and the relation of dielectric properties, therefore, the most also cannot predict its resonance from the composition of compound with structure
The microwave dielectric property such as frequency-temperature coefficient and quality factor, which greatly limits low temperature co-fired technology and microwave is many
The development of layer device.Explore with exploitation can low-temperature sintering have simultaneously 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 thirst for solving always but all the time
It is difficult to the difficult problem succeeded.
Summary of the invention
It is an object of the invention to provide and a kind of have good heat endurance and low-loss, low temperature sintering is ultralow simultaneously
Dielectric constant microwave dielectric ceramic material and preparation method thereof.
The chemical composition of the microwave dielectric ceramic material of the present invention is Li3Al2P3O12。
The preparation method step of this microwave dielectric ceramic material is:
(1) be 99.9%(percentage by weight by purity) more than Li2CO3、Al2O3And NH4H2PO4Starting powder press
Li3Al2P3O12Composition 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 ~ 900 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: Li3Al2P3O12Ceramic sintering temperature is low, and cost of material is low；Dielectric constant reaches dielectric constant
Reach 6.2～6.7, the temperature coefficient τ of its resonant frequencyƒLittle, temperature stability is good；Its quality factor q f value is up to 81000-
122000GHz, can be widely used for the manufacture of the microwave devices such as various medium substrate, resonator and wave filter, can meet low temperature altogether
The technology of burning technology and microwave multilayer device needs, and industrially has 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.By Li3Al2P3O12Powder with account for powder
Material quality 20% Ag powder mixing, compressing after, at 880 DEG C sinter 4 hours；X-ray diffraction material phase analysis and ESEM
Observe the Li all showing Ag with cubic garnet structure3Al2P3O12There is not chemical reaction, i.e. Li3Al2P3O12Can be with Ag electricity
The most low temperature co-fired.
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 low temperature sintering temperature-stable ultralow dielectric microwave dielectric ceramic, it is characterised in that described microwave is situated between
The chemical composition of electroceramics is: Li3Al2P3O12；
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、Al2O3And NH4H2PO4Starting powder press
Li3Al2P3O12Composition 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 ~ 900 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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| CN201410634371.5A CN104446433B (en) | 2014-11-12 | 2014-11-12 | Temperature-stable ultralow dielectric microwave dielectric ceramic Li3al2p3o12 |
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| CN106187148A (en) * | 2016-07-30 | 2016-12-07 | 桂林理工大学 | Lithio temperature-stable microwave dielectric ceramic Li8ga3p7o26 |
| CN106242551A (en) * | 2016-08-01 | 2016-12-21 | 桂林理工大学 | A kind of lithium-based compound Li9ga3p8o29application as temperature-stable microwave dielectric ceramic |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101870584A (en) * | 2010-05-12 | 2010-10-27 | 西安交通大学 | Molybdenum-based ultralow-temperature sintering microwave medium ceramic materials and preparation method thereof |
| CN103896572A (en) * | 2014-04-12 | 2014-07-02 | 桂林理工大学 | Temperature stable microwave dielectric ceramic Li3PO4 capable of being sintered at low temperature and preparation method of temperature stable microwave dielectric ceramic Li3PO4 |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101870584A (en) * | 2010-05-12 | 2010-10-27 | 西安交通大学 | Molybdenum-based ultralow-temperature sintering microwave medium ceramic materials and preparation method thereof |
| CN103896572A (en) * | 2014-04-12 | 2014-07-02 | 桂林理工大学 | Temperature stable microwave dielectric ceramic Li3PO4 capable of being sintered at low temperature and preparation method of temperature stable microwave dielectric ceramic Li3PO4 |
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Effective date of registration: 20201201 Address after: No.32, group 2, Yongxing Village, yong'anzhou Town, Gaogang District, Taizhou City, Jiangsu Province Patentee after: Chen Cheng Address before: 541004 the Guangxi Zhuang Autonomous Region Guilin Construction Road No. 12 Patentee before: GUILIN University OF TECHNOLOGY |
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Effective date of registration: 20210105 Address after: No.25-1, Gangcheng Road, dongyinggang Economic Development Zone, Hekou District, Dongying City, Shandong Province Patentee after: Shandong Xingqiang Chemical Industry Technology Research Institute Co., Ltd Address before: No.32, group 2, Yongxing Village, yong'anzhou Town, Gaogang District, Taizhou City, Jiangsu Province Patentee before: Chen Cheng |