CN103011810B - Low-temperature sintering can contain lithium garnet structure microwave dielectric ceramic Li 2ca 2biV 3o 12and preparation method thereof - Google Patents
Low-temperature sintering can contain lithium garnet structure microwave dielectric ceramic Li 2ca 2biV 3o 12and preparation method thereof Download PDFInfo
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Abstract
The invention discloses one and low-temperature sintering can contain lithium garnet structure microwave dielectric ceramic Li
2ca
2biV
3o
12and preparation method thereof.The constitutional chemistry formula of dielectric ceramic material is: Li
2ca
2biV
3o
12; (1) be the Li of more than 99.9% by purity
2cO
3, CaCO
3, Bi
2o
3and V
2o
3starting powder, by Li
2ca
2biV
3o
12constitutional chemistry formula weigh batching; (2) step (1) raw material wet ball-milling is mixed 12 hours, solvent is distilled water, pre-burning 6 hours in 650 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 700 ~ 750 DEG C of air atmosphere, sinter 4 hours; Described binding agent adopts mass concentration to be the polyvinyl alcohol solution of 5%, and dosage accounts for 3% of powder total amount.Pottery prepared by the present invention is good at 700 ~ 750 DEG C of sintering, and its specific inductivity reaches 37 ~ 43, and quality factor q f value is up to 65000-94000GHz, 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 the microwave device such as dielectric resonator, wave filter used in microwave frequency, and the dielectric ceramic material of ceramic condenser or thermo-compensation capacitor and preparation method thereof.
Background technology
Microwave dielectric ceramic refers to and to be applied in microwave frequency band (mainly UHF, 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, 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, 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: the relative permittivity e that (1) is high
rbe beneficial to the miniaturization of device, general requirement e
r>=20; (2) high quality factor q value or dielectric loss tan δ to reduce noise, general requirement Qf>=3000 GHz; (3) the temperature factor t of resonant frequency
flittle of as far as possible to ensure the thermostability that device has had, general requirement-10/ DEG C≤t
f≤+10 ppm/ DEG C; From late 1930s, just someone attempts dielectric substance to be applied to microwave technology in the world.
According to relative permittivity e
rsize from use frequency range different, usually the microwave-medium ceramics be developed and developing can be divided into 3 classes.
(1) low e
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=25 ~ 30, Q=(1 ~ 2) × 10
4(under the GHz of f>=10), τ
?≈ 0.Be mainly used in the microwave communication equipments such as the direct broadcasting satellite of f >=8 GHz as dielectric resonance device.
(2) 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 ~ 40, Q=(6 ~ 9) × 10
3(under f=3 ~-4GHz), t
?≤ 5 ppm/ ° C.Be mainly used in microwave military radar in 4 ~ 8 GHz range of frequency and communication system as dielectric resonance device.
(3) 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, 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 Ag, the low melting point metals such as Cu burn formation laminated ceramic capacitor altogether, in recent years, along with LTCC Technology (Low Temperature Co-fired Ceramics, 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, but, still more limited for the system for low fever's microwave-medium ceramics, which greatly limits the development of low temperature co-fired technology and microwave multilayer device, we are to garnet structure type pottery NaCa
2(Mg
1-xzn
x)
2v
3o
12, LiCa
3mg
1-xzn
xv
3o
12carried out sintering characteristic and Study on microwave dielectric property, found that such pottery have excellent comprehensive microwave dielectric property simultaneously sintering temperature lower than 960
°c, can be widely used in various medium substrate, manufacture that resonance plays the microwave device such as device, wave filter, can meet the technology needs of low temperature co-fired technology and microwave multilayer device, in order to reduce sintering temperature further, we find to consist of garnet structure oxide ceramics Li
2ca
2biV
3o
12compare NaCa
2(Mg
1-xzn
x)
2v
3o
12, LiCa
3mg
1-xzn
xv
3o
12deng the sintering temperature that tool is lower, there is more high-k and the temperature factor of resonant frequency of nearlyer zero simultaneously, therefore there is more excellent over-all properties.
Summary of the invention
The object of this invention is to provide one and low-temperature sintering can contain lithium garnet structure microwave dielectric ceramic Li
2ca
2biV
3o
12and preparation method thereof.
What the present invention relates to can low-temperature sintering containing the constitutional chemistry formula of lithium garnet structure microwave dielectric ceramic be: Li
2ca
2biV
3o
12.
Above-mentionedly can low-temperature sintering containing preparation method's concrete steps of lithium garnet structure microwave dielectric ceramic be:
(1) be the Li of more than 99.9% by purity
2cO
3, CaCO
3, Bi
2o
3and V
2o
3starting powder press Li
2ca
2biV
3o
12chemical formula weigh batching;
(2) step (1) raw material wet ball-milling is mixed 12 hours, solvent is distilled water, pre-burning 6 hours in 650 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 700 ~ 750 DEG C of air atmosphere, sinter 4 hours; Described binding agent adopts mass concentration to be the polyvinyl alcohol solution of 5%, and dosage accounts for 3% of powder total amount.
Pottery prepared by the present invention is good at 700 ~ 750 DEG C of sintering, and its specific inductivity reaches 37 ~ 43, and quality factor q f value is up to 65000-94000GHz, and temperature coefficient of resonance frequency is little, industrially has great using value.
Embodiment
Embodiment:
Table 1 shows 4 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 that various dielectric resonance plays the microwave device such as device, wave filter, can meet the technology needs of the system such as mobile communication, satellite communications.
The present invention is never limited to above embodiment, have with the element of the analog structures such as Bi and chemical property as La, Eu, Y, Ce, Gd, Tb, Dy, Ho, Tm, Yb and Lu etc. also can make with analogous crystalline structure of the present invention and performance dielectric ceramic.
Table 1:
Claims (1)
1. contain lithium garnet structure composite oxides as an application for microwave dielectric ceramic, it is characterized in that the constitutional chemistry formula of described composite oxides is: Li
2ca
2biV
3o
12;
Preparation method's step of described composite oxides is:
(1) be the Li of more than 99.9% by purity
2cO
3, CaCO
3, Bi
2o
3and V
2o
3starting powder press Li
2ca
2biV
3o
12chemical formula weigh batching;
(2) step (1) raw material wet ball-milling is mixed 12 hours, solvent is distilled water, pre-burning 6 hours in 650 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 700 ~ 750 DEG C of air atmosphere, sinter 4 hours; Described binding agent adopts mass concentration to be the polyvinyl alcohol solution of 5%, and dosage accounts for 3% of powder total amount.
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CN103496983A (en) * | 2013-10-01 | 2014-01-08 | 桂林理工大学 | Low temperature sintered microwave dielectric ceramic BiCaVO5 and preparation method thereof |
CN104003719B (en) * | 2014-05-17 | 2016-01-13 | 桂林理工大学 | Low temperature sintering microwave dielectric ceramic LiTi 2v 3o 12and preparation method thereof |
CN104557020B (en) * | 2014-12-27 | 2016-09-28 | 桂林理工大学 | A kind of sintered at ultra low temperature ultralow dielectric microwave dielectric ceramic and preparation method thereof |
CN104649665A (en) * | 2014-12-28 | 2015-05-27 | 桂林理工大学 | Microwave medium ceramic Li2La3NdV2O12 with near zero temperature coefficient of resonant frequency |
JP6744143B2 (en) | 2015-06-15 | 2020-08-19 | スカイワークス ソリューションズ, インコーポレイテッドSkyworks Solutions, Inc. | Synthetic garnet material, modified synthetic garnet composition, and method of making synthetic garnet |
CN105236968A (en) * | 2015-09-07 | 2016-01-13 | 桂林理工大学 | Low-loss and high-thermal-stability ultralow-dielectric-constant microwave dielectric ceramic LiCaEuV2O8 |
CN105218096B (en) * | 2015-09-22 | 2017-08-29 | 中国工程物理研究院化工材料研究所 | A kind of transparent YAG microwave dielectric ceramic materials of high Q and its application |
US20180166763A1 (en) | 2016-11-14 | 2018-06-14 | Skyworks Solutions, Inc. | Integrated microstrip and substrate integrated waveguide circulators/isolators formed with co-fired magnetic-dielectric composites |
US11081770B2 (en) | 2017-09-08 | 2021-08-03 | Skyworks Solutions, Inc. | Low temperature co-fireable dielectric materials |
US11603333B2 (en) | 2018-04-23 | 2023-03-14 | Skyworks Solutions, Inc. | Modified barium tungstate for co-firing |
US11565976B2 (en) | 2018-06-18 | 2023-01-31 | Skyworks Solutions, Inc. | Modified scheelite material for co-firing |
Citations (1)
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CN1238317A (en) * | 1999-06-14 | 1999-12-15 | 西安交通大学 | Low-temp sintered high-performance and-frequency dielectric ceramic |
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CN102584208A (en) * | 2012-02-18 | 2012-07-18 | 桂林理工大学 | Low-temperature sinterable microwave dielectric ceramic BiZn2VO4 and preparation method thereof |
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CN1238317A (en) * | 1999-06-14 | 1999-12-15 | 西安交通大学 | Low-temp sintered high-performance and-frequency dielectric ceramic |
Non-Patent Citations (1)
Title |
---|
邱克辉等.Ca2Li2BiV3O12:Eu3+荧光粉的制备和发光性能.《发光学报》.2012,第33卷(第2期),第161-165页. * |
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