CN110256071A - A kind of LTCC microwave dielectric ceramic materials and preparation method thereof - Google Patents
A kind of LTCC microwave dielectric ceramic materials and preparation method thereof Download PDFInfo
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Abstract
Present invention relates particularly to a kind of simple LTCC microwave dielectric ceramic materials of formula and preparation method thereof.Chemical composition are as follows: (1-x) Li4Ti5O12+xNb2TiO7+ ywt%CeO2, wherein 0.3≤x≤0.7,0≤y≤1.The present invention is a kind of inexpensive, simple process microwave-medium ceramics, significantly reduce production cost, improve production efficiency, it is a kind of with low temperature sintering and the small, temperature coefficient of loss is bordering on zero microwave dielectric ceramic materials, the microwave devices such as capacitor, dielectric resonator, filter and duplexer suitable for LTCC, low in raw material price, process route are simple and easy.
Description
Technical field
The invention belongs to electronic information function material and device arts, and in particular to a kind of LTCC is made pottery with microwave-medium
Ceramic material and preparation method thereof.
Background technique
The rapid development of present mobile communication, push all kinds of microwave mobile communication terminal devices to miniaturization, lightweight,
Multifunction and cost effective direction are fast-developing.With low-temperature co-fired ceramics (Low Temperature Co-fired
Ceramic, LTCC) multi-layer structure design based on technology can effectively reduce device volume, and it is to realize component to small-sized
Change, integrated and modular important channel.LTCC technology use multilayered structure, it is desirable that microwave dielectric material can with it is highly conductive
(961 DEG C) realization cofirings of rate and cheap silver electrode.It is therefore desirable to for using the microwave dielectric material on microwave device
Sintering temperature will be at 950 DEG C or less.Low melting point oxide or glass sintering auxiliary agent are added to reduce the burning of microwave dielectric material
Junction temperature is the method that one of the most common type reduces sintering temperature.Li4Ti5O12Series microwave dielectric ceramic be recently just developed it is new
Type microwave-medium ceramics, with good microwave dielectric property, but sintering temperature is higher, temperature coefficient of resonance frequency compared with
Difference cannot apply in LTCC technology.The invention is to solve the problems, such as this, is applied to it in LTCC technique.
Summary of the invention
Have the characteristics that low temperature sintering, Qf high and rate of temperature change are low the object of the present invention is to provide a kind of
LTCC microwave dielectric ceramic materials and preparation method thereof.
The purpose of the present invention is what is be achieved through the following technical solutions: a kind of LTCC microwave dielectric ceramic materials, by leading
Crystalline phase material and doping phase material are made through ball milling mixing, pre-burning, doping ball milling, dries pulverizing.The wherein main crystal phase material
For Li2CO3, mass percent is 20~40%, Nb2O5Mass percent is 10~20%, TiO2Mass percent be 50~
70%;The doping phase material CeO2, mass percent is 0~1%.
Li in the main crystal phase material4Ti5O12、Nb2TiO7Between molar ratio be 1-x:x, x be 0.3~0.7.
The doping phase material is oxide CeO2, mass percent is 0~1%.
A kind of preparation method of LTCC microwave dielectric ceramic materials, includes the following steps:
(1), prepared by main crystal phase material, weighs lightweight Li respectively in molar ratio2CO3、Nb2O5、TiO2, in material: ball: the ratio of water
1:2:0.8 carries out ball milling, and after drying, pre-burning at high temperature synthesizes main crystal phase material.
(2), the main crystal phase material after pre-burning presses 0~1% doping phase material CeO after crushing2, by the condition of step 1
Carry out secondary ball milling, after drying, crushing packing.
Microwave dielectric ceramic materials of the invention at being grouped as are as follows: (1-x) Li4Ti5O12+xNb2TiO7+ ywt%
CeO2, wherein 0.3≤x≤0.7,0≤y≤1.
The crucial group that the present invention forms microwave dielectric ceramic materials becomes (1-x) Li4Ti5O12+xNb2TiO7+ ywt%
CeO2, lithium, niobium, titanium and Ce elements are contained in formula components, prepare raw material Li, Nb of this microwave dielectric ceramic materials, Ti,
Ce is salt and oxide containing these elements.Wherein, doped chemical cerium is the resonance frequency in order to adjust microwave dielectric ceramic materials
Rate temperature coefficient τf, reduce sintering temperature.
Primary focus of the invention is the component prescription of microwave dielectric ceramic materials, can basis in actual application
It needs to adjust accordingly synthetic method and production technology, flexibility is big.Solid reaction process, colloidal sol-can be used in synthetic method
Gel method, coprecipitation, the synthetic method of vapour deposition process or other ceramic materials are realized.The present invention, which selects, is suitable for industry greatly
The solid reaction process of production, being conducive to production cost reduces.
The detection of microwave dielectric ceramic materials characteristic of the invention is to use to be pressed into disk, high temperature sintering, burning infiltration silver electricity
Pole measures the characterisitic parameter of tile with HP4291B impedance analyzer.
The characteristic and Heterosis of microwave dielectric ceramic materials of the present invention exist: 1. material composition is simple, raw material
Compare it is abundant, it is environmental-friendly;2. calcined temperature is lower in preparation process, production cost is reduced;3. material is using elemental cerium as mixing
Miscellaneous element;4. by adjusting metatitanic acid content of niobium tunable dielectric constant and rate of temperature change;5. being contained by cerium in modifying ingredients composition
Amount, adjustable temperature coefficient of resonance frequency reduce sintering temperature.
The electrical property of microwave dielectric ceramic materials of the present invention can realize following parameter request: dielectric constant is 62 ± 2,
Qf >=40000GHz, τf≈0±10ppm/℃。
The invention has the beneficial effects that: preparation method simple process, production cost is low, easy to accomplish, and sintering temperature is low,
The Qf value for improving material, reduces the τ of productfValue, the requirement being able to satisfy under LTCC microwave condition.
The contents of the present invention are further described with the following Examples.Following embodiment only meets the technology of the present invention
Several examples of content do not illustrate that present invention is limited only to contents described in following examples.The ingredient that focuses on of the invention is matched
Side, the raw material, process and step can be adjusted correspondingly according to actual production conditions, and flexibility is big.
Fig. 1 is the schematic diagram of internal structure of microwave dielectric ceramic materials of the present invention.
Specific embodiment
The present invention uses the Li of purity assay2CO3、Nb2O5、TiO2Principal crystalline phase is prepared for raw material, is the CeO of 4N with purity2
It is doped, specific embodiment is as follows: weighing ingredient by table 1, mixture is put into stirring-type ball grinder, by pellet water quality
Amount is than 1:2:0.8, and ball milling 2~6 hours, revolving speed was 260 revs/min.Granularity is controlled in D50It is within=1.2 μm, ball milling is mixed
Material is put in 100 DEG C of baking oven drying, smashes it through 40 meshes, 880 DEG C/4H condition pre-burning is pressed in chamber type electric resistance furnace, after crushing
It is spare to cross 40 meshes;Secondary ball milling is carried out by above-mentioned condition, granularity control is at 0.8 μm hereinafter, dries pulverizing is sieved, with manual pressure
Machine 20MPa forms outer diameter Φ 12.2mm, the disk of thickness 2mm.Green compact sample is placed in sintering furnace, under the conditions of 950 DEG C/3H,
Sinter tile sample into, two sides coats silver paste, burning infiltration under the conditions of 850 DEG C/10M, by HP4291B impedance analyzer to sample into
Row performance test.
The specific embodiment of the invention is shown in Table 2 at porcelain density, dielectric properties result in detail.
Each example list of ingredients of table 1.
The properties of sample of each example of table 2.
Claims (6)
1. a kind of LTCC microwave dielectric ceramic materials and preparation method thereof are mixed by main crystal phase material and doping phase material through ball milling
Conjunction, pre-burning, doping ball milling, dries pulverizing are made;Wherein: the main crystal phase material is Li2CO3Mass percent is 20~40%,
Nb2O5Mass percent is 10~20%, TiO2Mass percent is 50~70%;The doping phase material CeO2, quality percentage
Than being 0~1%.
2. a kind of LTCC microwave dielectric ceramic materials and preparation method thereof according to claim 1, it is characterised in that institute
It states in main crystal phase material, Li4Ti5O12、Nb2TiO7Between molar ratio be 1-x:x, x be 0.3~0.7.
3. a kind of LTCC microwave dielectric ceramic materials and preparation method thereof according to claim 1, it is characterised in that institute
Stating doping phase material is oxide CeO2, mass percent is 0~1%.
4. a kind of LTCC microwave dielectric ceramic materials and preparation method thereof according to claim 1, it is characterised in that be situated between
The preparation method of ceramics, includes the following steps:
(1), prepared by main crystal phase material, weighs lightweight Li respectively in molar ratio2CO3、Nb2O5、TiO2, in material: ball: the ratio 1 of water:
2:0.8 carries out ball milling, and after drying, pre-burning at high temperature synthesizes main crystal phase material;(2), the main crystal phase material after pre-burning crushes
0~1% doping phase material CeO is pressed afterwards2, secondary ball milling, after drying, crushing packing are carried out by the condition of step 1.
5. a kind of LTCC microwave dielectric ceramic materials and preparation method thereof according to claim 1, it is characterised in that be situated between
Ceramics at being grouped as are as follows: (1-x) Li4Ti5O12+xNb2TiO7+ ywt% CeO2, wherein 0.3≤x≤0.7,0≤y
≤1。
6. a kind of LTCC microwave dielectric ceramic materials and preparation method thereof according to claim 1, it is characterised in that this
The crucial group of invention medium ceramic material becomes (1-x) Li4Ti5O12+xNb2TiO7+ ywt% CeO2, contain in formula components
Lithium, niobium, titanium and Ce elements, raw material Li, Nb, Ti, the Ce for preparing this microwave dielectric ceramic materials are the salt containing these elements
And oxide;Wherein, doped chemical cerium is the temperature coefficient of resonance frequency τ in order to adjust microwave dielectric ceramic materialsf, reduce and burn
Junction temperature.
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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US20030211931A1 (en) * | 2002-05-13 | 2003-11-13 | Hyun-Jai Kim | Low temperature co-firing ceramic (LTCC) composition for microwave frequency |
CN101224977A (en) * | 2008-01-18 | 2008-07-23 | 西安交通大学 | Low-temperature sintered LTCC microwave dielectric ceramics material and preparation method thereof |
CN103601487A (en) * | 2013-11-29 | 2014-02-26 | 电子科技大学 | (SrCa)TiO3-LaAlO3-based microwave dielectric ceramic material and preparation method thereof |
CN105314978A (en) * | 2015-12-05 | 2016-02-10 | 桂林理工大学 | Lithium-based high-performance microwave dielectric ceramic material and preparation method thereof |
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2019
- 2019-06-19 CN CN201910529161.2A patent/CN110256071A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20030211931A1 (en) * | 2002-05-13 | 2003-11-13 | Hyun-Jai Kim | Low temperature co-firing ceramic (LTCC) composition for microwave frequency |
CN101224977A (en) * | 2008-01-18 | 2008-07-23 | 西安交通大学 | Low-temperature sintered LTCC microwave dielectric ceramics material and preparation method thereof |
CN103601487A (en) * | 2013-11-29 | 2014-02-26 | 电子科技大学 | (SrCa)TiO3-LaAlO3-based microwave dielectric ceramic material and preparation method thereof |
CN105314978A (en) * | 2015-12-05 | 2016-02-10 | 桂林理工大学 | Lithium-based high-performance microwave dielectric ceramic material and preparation method thereof |
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