CN106986636A - A kind of low temperature sintering microwave ceramic material and preparation method thereof - Google Patents

A kind of low temperature sintering microwave ceramic material and preparation method thereof Download PDF

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CN106986636A
CN106986636A CN201710236375.1A CN201710236375A CN106986636A CN 106986636 A CN106986636 A CN 106986636A CN 201710236375 A CN201710236375 A CN 201710236375A CN 106986636 A CN106986636 A CN 106986636A
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李波
郑景国
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University of Electronic Science and Technology of China
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Abstract

The invention belongs to electric function ceramic and component technical field, it is related to Microwave Device and Circuitry, a kind of low temperature sintering microwave ceramic material and preparation method thereof is specifically provided, to the shortcoming for overcoming existing low temperature sintering microwave ceramic temperature coefficient not return to zero；The chemical expression of microwave ceramic material of the present invention is：Ca5+ACo4+BV6+CO24- XCaTiO3, wherein A+B+C=0.05,0.05≤A≤0,0.05≤B≤0,0.05≤C≤0,2wt%<X≤10wt%；The microwave ceramics can altogether be burnt with argent and not with the biochemical reaction of silver hair, and can realize that temperature coefficient of resonance frequency is：10ppm/ DEG C~+10ppm/ DEG C, i.e. zero-temperature coefficient；Simultaneously, the material possesses the low characteristic of sintering temperature, it is not required to add any sintering aid, it effectively prevent the generation that sintering aid causes its dielectric properties to deteriorate, and keep higher consistency and porcelain body intensity, preparation technology is simple and environmentally-friendly to be saved, repeats and with low cost, it is easy to accomplish industrialized production.

Description

A kind of low temperature sintering microwave ceramic material and preparation method thereof
Technical field
The invention belongs to electric function ceramic and component technical field, especially Microwave Device and Circuitry, it is related to one kind Low temperature sintering microwave ceramic material and preparation method thereof.
Background technology
The fast development of microelectronic component and integrated device proposes high requirement to electronics miniaturization, lightweight, Single active device is integrated can not to meet generation application, and passive device is had necessarily become smaller as a kind of trend, but tradition The Metal cavity of large volume used makes the integrated of microstrip circuit become difficult.Microwave Multichip Module (MMCM) module is because having It is lightweight, small volume, cost is low and the high technical characterstic of reliability and be widely used, realizing the effective way of this technology is Develop multiple field element.LTCC (Low Temperature Co-fired Ceramics, LTCC) technology is because of it There is higher integration density, preferable high frequency characteristics, have become realize Current electronic component it is integrated one Plant major way.The Miltilayer wiring structure that LTCC technology is used is a kind of passive device integration and passive device of 3 D stereo assembling Part hybrid integrated technology, can realize that passive element (resistance, electric capacity, inductance, wave filter) is integrated with transmission line, again can surface Mount IC, for realization during miniaturization, the modularization of multi-functional and improve signal reliability in terms of play it is important Role.
The interconnection conductors that LTCC technology is used typically have the silver metal of superior electrical conductivity, and its fusing point is about 961 DEG C, and this is just It is required that applying the ceramic material in LTCC technology to have to the densified sintering product below 950 DEG C, in addition, applying in LTCC technology Microwave ceramic material should also have the characteristics that：(1) suitable dielectric constant is to be conducive to the miniaturization of device；(2) it is high Quality factor require Q × f >=20000GHz to reduce loss, typically；(3) nearly zero temperature coefficient (10~+10ppm/ DEG C) with Be conducive to temperature stability.However, various high temperature sintering microwave ceramics (is sintered and caused to meet LTCC temperature requirement Close temperature is less than 950 DEG C) it must all add sintering aid (B2O3, glass and V2O5Deng low melting point oxide), such as in Ohsato H,Ohhashi T,Kato H,et al.Microwave Dielectric Properties and Structure of the Ba6-3xSm8+2xTi18O54Solid Solutions[J].Japanese Journal of Applied Physics,1995,34 (1):Reported in 187-191, Ba6-3xSm8+2xTi18O54By adding 0.5wt%B2O3Sintering temperature is dropped to from 1733K 1473K, while quality factor and dielectric constant are also reduced, here it is typically sacrificing microwave dielectric property exchanges low-temperature sintering for Case.It follows that although sintering aid can play the effect that drop is burnt, the addition of sintering aid can deteriorate its microwave dielectric property Can, while reducing consistency and porcelain body intensity；The structure that addition sintering aid is formed is difficult to control, and preparation technology is relative complex, Usual sintering aid must all be manufactured separately, and such as pass through glass melting process, the complexity of technique is not only increased in the process, And mass energy need to be expended and add energy consumption.Therefore low temperature sintering microwave ceramic is developed into a kind of trend.
Vanadic acid salt system is a kind of new LTCC microwave dielectric materials, and not only sintering temperature is low, and high with Q × f values Advantage, it is little by little of interest by people in recent years.For example in Journal of the American Ceramic Society,2013,96(6):1691-1693《Novel Series of Low‐Firing Microwave Dielectric Ceramics:Ca5A4(VO4)6(A2+=Mg, Zn)》Report, Ca5Zn4(VO4)6And Ca5Mg4(VO4)6Microwave ceramics at 725 DEG C and The microwave dielectric property sintered at 800 DEG C：Dielectric constant 11.7 and 9.2, quality factor q × f=49400GHz and 53300GHz, - 83ppm/ DEG C and -50ppm/ DEG C of temperature coefficient；In Journal of Materials Science:Materials in Electronics 2016,27(7):7292-7296《Microwave dielectric properties of low temperature sintering Ca5Mn4(VO4)6》Report, Ca5Mn4(VO4)6Microwave dielectric property：Dielectric constant 11.7, Quality factor q × f=33800GHz, -70ppm/ DEG C of temperature coefficient.Although above-mentioned vanadate system microwave ceramic disclosure satisfy that LTCC temperature requirement (densified sintering product temperature is less than 950 DEG C), but the requirement of nearly zero temperature coefficient, serious limitation can not be met It is in the application of microwave device, and the microwave ceramics that thus works out the requirements for meeting LTCC technology has become urgently The need for.
The content of the invention
It is existing to overcome it is an object of the invention to provide a kind of low temperature sintering microwave ceramic material and preparation method thereof The shortcoming that low temperature sintering microwave ceramic temperature coefficient does not return to zero；The chemical expression of the microwave ceramic material is：Ca5+ACo4+BV6+ CO24- XCaTiO3, wherein A+B+C=-0.05, -0.05≤A≤0, -0.05≤B≤0, -0.05≤C≤0,0<X≤15；Should Microwave ceramics can altogether be burnt with argent and not with the biochemical reaction of silver hair, and can realize that temperature coefficient of resonance frequency is：- 10ppm/ DEG C~+10ppm/ DEG C, meanwhile, preparation technology is simple, cost is low, repeats, be easy to industrialized production.
To achieve the above object, the technical solution adopted by the present invention is：
A kind of low temperature sintering microwave ceramic material, it is characterised in that the chemical expression of the microwave ceramic material is： Ca5+ACo4+BV6+CO24- XCaTiO3, wherein A+B+C=-0.05, -0.05≤A≤0, -0.05≤B≤0, -0.05≤C≤0, 2wt%<X≤10wt% (especially 4wt%<X≤8wt%).
The principal crystalline phase of the microwave-medium ceramics is Ca5Co4(VO4)6, secondary crystalline phase is CaTiO3。
The preparation method of above-mentioned low temperature sintering microwave ceramic material, comprises the following steps：
Step 1：With CaCO3、Co2O3、V2O5And CaTiO3For raw material, according to mol ratio CaCO3：Co2O3：V2O5=5+A：4+ B：6+C carries out dispensing, well mixed to obtain compound, wherein, A+B+C=-0.05, -0.05≤A≤0, -0.05≤B≤0, - 0.05≤C≤0,2wt%<X≤10wt%；
Step 2：Step 1 gained compound is sequentially passed through into ball milling, drying, sieving, obtains drying powder；And in 750~ 4~6h of pre-burning, obtains Preburning material at a temperature of 850 DEG C；
Step 3：Step 2 gained Preburning material is sequentially passed through into ball milling, drying, sieving again, secondary ball abrasive material is obtained；
Step 4：The binding agent PVA that step 3 gained secondary ball abrasive material is added into 5~10wt% is granulated after mixing, is molded To green compact；
Step 5：By step 4 gained green compact temperature be 900~950 DEG C, atmosphere be to sinter 1~7h under conditions of air, Obtain the microwave ceramic material.
Further, in the step 2 and step 3, Ball-milling Time is：4~7h, drying temperature is：80~100 ℃。
In the step 4, granulation size is 100~250 mesh, in 20MPa forming under the pressure.
The beneficial effects of the present invention are：
The present invention provides a kind of low temperature sintering microwave ceramic material and preparation method thereof, and the microwave ceramic material can be realized Temperature coefficient of resonance frequency is：- 10ppm/ DEG C~+10ppm/ DEG C, i.e. zero-temperature coefficient；The material possesses the low spy of sintering temperature Property (sintering temperature<950 DEG C), it is not required to add any sintering aid, effectively prevent the hair that sintering aid causes its dielectric properties to deteriorate It is raw, and keep higher consistency and porcelain body intensity；Meanwhile, it effectively prevent the multiphase structure that is formed of addition sintering aid and be difficult to The problems such as control, preparation technology complicated (sintering aid must be manufactured separately, and such as pass through glass melting process)；To sum up, the present invention is carried For a kind of zero-temperature coefficient low-temperature sintering microwave medium, meanwhile, the simple and environmentally-friendly energy-conservation of microwave ceramic material preparation technology, again Answer and with low cost, it is easy to accomplish industrialized production.
Brief description of the drawings
Fig. 1 is that embodiment 1 is prepared into microwave ceramic material Ca5+ACo4+BV6+CO24- XCaTiO3XRD diffraction analysis figures.
Fig. 2 is that embodiment 1 is prepared into microwave ceramic material Ca5+ACo4+BV6+CO24- XCaTiO3SEM electron microscopes Figure.
Embodiment
With reference to specific embodiment, the present invention is further elaborated：
1~embodiment of embodiment 5
The chemical expression of offer microwave-medium is in above-described embodiment：
The microwave ceramics specific implementation step that these embodiments are made is as follows：Ca5+ACo4+BV6+CO24- XCaTiO3, its In, A=B=0, C=-0.05, X=6wt%；The specific preparation process of the microwave ceramic material is as follows：
Step 1：Raw materials of Ca CO is weighed according to being matched described in claim 1 according to the chemical general formula of invention material3、Co2O3、 V2O5And CaTiO3Carry out dispensing and be mixed to get compound；
Step 2：, by ball milling 7h, it will be dried at 100 DEG C by step 1 gained compound and cross 40 mesh sieves, in 775 DEG C of temperature The lower pre-burning 3h of degree, obtains Preburning material；
Step 3：Obtained Preburning material is subjected to secondary ball milling 7h, obtained ball milling material in being dried at 100 DEG C after ball milling is complete Secondary ball abrasive material；
Step 4：Obtained secondary ball abrasive material is added to the binding agent that 5~10wt% is added equivalent to the secondary ball abrasive material Granulated after PVA mixing, granulation size Control obtains green compact in 100~250 mesh, and in 20MPa forming under the pressure；
Step 5：The green compact that step 4 is obtained temperature be 900~950 DEG C, atmosphere be sintering 1 under conditions of air~ 7h, obtains final required microwave ceramics.
Step 6：Test：According to Hakki-Coleman dielectric resonance methods, with the microwave-medium of Network Analyzer test sample Performance.
The specific composition of 1~embodiment of embodiment 5 is constituted, technological parameter and microwave dielectric property are as shown in the table：
The foregoing is only a specific embodiment of the invention, any feature disclosed in this specification, except non-specifically Narration, can alternative features equivalent by other or with similar purpose replaced；Disclosed all features or all sides Method or during the step of, in addition to mutually exclusive feature and/or step, can be combined in any way.

Claims (5)

1. a kind of low temperature sintering microwave ceramic material, it is characterised in that the chemical expression of the microwave ceramic material is：Ca5+ ACo4+BV6+CO24- XCaTiO3, wherein A+B+C=-0.05, -0.05≤A≤0, -0.05≤B≤0, -0.05≤C≤0, 2wt%<X≤10wt%.
2. the low temperature sintering microwave ceramic material as described in claim 1, it is characterised in that the principal crystalline phase of the microwave ceramic material For Ca5Co4(VO4)6, secondary crystalline phase is CaTiO3。
3. the preparation method of low temperature sintering microwave ceramic material, comprises the following steps as described in claim 1：
Step 1：With CaCO3、Co2O3、V2O5And CaTiO3For raw material, according to mol ratio CaCO3：Co2O3：V2O5=5+A：4+B：6+ C carries out dispensing, well mixed to obtain compound, wherein, A+B+C=-0.05, -0.05≤A≤0, -0.05≤B≤0, -0.05 ≤ C≤0,2wt%<X≤10wt%；
Step 2：Step 1 gained compound is sequentially passed through into ball milling, drying, sieving, obtains drying powder；And in 750~850 DEG C At a temperature of 4~6h of pre-burning, obtain Preburning material；
Step 3：Step 2 gained Preburning material is sequentially passed through into ball milling, drying, sieving again, secondary ball abrasive material is obtained；
Step 4：Granulation, shaping are given birth to after the binding agent PVA that step 3 gained secondary ball abrasive material is added into 5~10wt% is mixed Base；
Step 5：By step 4 gained green compact temperature be 900~950 DEG C, atmosphere be to sinter 1~7h under conditions of air, obtain The microwave ceramic material.
4. the preparation method of low temperature sintering microwave ceramic material as described in claim 3, it is characterised in that the step 2 and step In rapid 3, Ball-milling Time is：4~7h, drying temperature is：80~100 DEG C.
5. the preparation method of low temperature sintering microwave ceramic material as described in claim 3, it is characterised in that in the step 4, make Particle size is 100~250 mesh, in 20MPa forming under the pressure.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108689710A (en) * 2018-05-24 2018-10-23 电子科技大学 A kind of low-temperature sintering Ca5Mn4V6O24Microwave dielectric material and preparation method thereof
CN111548158A (en) * 2020-05-19 2020-08-18 电子科技大学 Ultralow temperature sintering microwave medium composite material Sr1-xCaxV2O6And method for preparing the same

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
GUOGUANG YAO.ETC: "Low-temperature sintering and microwave dielectric properties of Ca5C4（VO4）6 ceramics", 《JOURNAL OF THE EUROPEAN CERAMIC SOCIETY》 *
张黄莉等: ""（1-x）ca5zn4（vo4）6-xca0.8sr0.2tio3陶瓷微波介电性能研究"", 《西安邮电大学学报》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108689710A (en) * 2018-05-24 2018-10-23 电子科技大学 A kind of low-temperature sintering Ca5Mn4V6O24Microwave dielectric material and preparation method thereof
CN111548158A (en) * 2020-05-19 2020-08-18 电子科技大学 Ultralow temperature sintering microwave medium composite material Sr1-xCaxV2O6And method for preparing the same
CN111548158B (en) * 2020-05-19 2022-06-03 电子科技大学 Ultralow temperature sintering microwave medium composite material Sr1-xCaxV2O6And method for preparing the same

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