CN106927826A - A kind of intermediary's microwave-medium ceramics and preparation method thereof - Google Patents
A kind of intermediary's microwave-medium ceramics and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of intermediary's microwave-medium ceramics and preparation method thereof, the chemical formula of the ceramic material is Nd0.34Ca0.396Sr0.264Al0.34Ti0.66O3, dielectric constant is 42~43, and quality factor q × f is 30000~40000GHz.Method of the present invention preparation process is simple, process is pollution-free, and repeatability is good, and obtained middle-dielectric constant microwave-medium ceramic material microwave dielectric property is excellent, has broad application prospects.
Description
Technical field
The invention belongs to microwave-medium ceramics technical field, and in particular to a kind of intermediary's microwave-medium ceramics and preparation method thereof.
Background technology
In recent years, developing rapidly with mechanics of communication, the demand to microwave device is also growing.Microwave-medium ceramics
Have the advantages that lossy microwave is low, dielectric constant is high and frequency-temperature coefficient is small, can both meet the mobility, just of communication equipment
The property taken, miniaturization, the requirement of miniaturization, can meet again has high-performance, the requirement of high reliability working characteristics in microwave range,
Obtain extensive concern.
The microwave dielectric ceramic with medium dielectric constant in microwave system is applied to, its Essential Performance Requirements is：Dielectric constant=30~
60, temperature coefficient of resonance frequency=- 5~5ppm/ DEG C, quality factor q × f >=5000GHz.NdAlO3With quality factor high
(Q × f=68000GHz), permittivity εr(εr=23) and negative temperature coefficient of resonance frequency (τ f=-44ppm/ DEG C).Can be with
By CaTiO of the addition with larger positive temperature coefficient of resonance frequency3(τ f=1534ppm/ DEG C) is adjusted.B.Jancar etc.
Research (1-x) NdAlO3-x CaTiO3The microwave dielectric property of system ceramics.The present invention is used using above-mentioned experiment thought
Ca0.4Sr0.6TiO3(τ f=1200ppm/ DEG C) adjusts NdAlO3Temperature coefficient has obtained a new microwave-medium ceramics
Nd0.34Ca0.396Sr0.264Al0.34Ti0.66O3It has excellent microwave dielectric property εr=43, Q × f=33000GHz, τ f=1.5
ppm/℃
The content of the invention
For the disadvantages described above of prior art, it is an object of the present invention to provide in a kind of process is simple, stable performance
Dielectric microwave media ceramic and preparation method thereof.Microwave-medium ceramics of the invention, preparation process is simple, repeatability are good and micro-
Ripple dielectric properties are excellent.
Here, the present invention provides a kind of intermediary's microwave-medium ceramics, the composition of intermediary's microwave-medium ceramics is
Nd0.34Ca0.396Sr0.264Al0.34Ti0.66O3, the dielectric constant of intermediary's microwave-medium ceramics is 42~43, quality factor q f
It is 31000~40000GHz, temperature coefficient of resonance frequency is 1ppm/ DEG C~3ppm/ DEG C.
Present invention also offers a kind of preparation method of above-mentioned middle-dielectric constant microwave-medium ceramic material, the preparation method bag
Include：
(1) chemical raw material calcium source, barium source, titanium source, neodymium source and silicon source are weighed into dispensing, a ball milling by the chemical formula respectively
Drying and screening after 12~24 hours, obtains original powder；
(2) by gained original powder at 1350 DEG C~1450 DEG C after pre-burning 4~6 hours, secondary ball milling 6~12 hours is dried
To preburning powdered material；
(3) to adding binding agent in gained preburning powdered material and granulating, it is pressed into idiosome；
(4) gained idiosome is sintered 4~12 hours at 1450~1550 DEG C, obtains described intermediary's microwave dielectric ceramic materials.
In the present invention, the calcium source can be CaCO3, the barium source can be SrCO3, the titanium source can be TiO2, the neodymium
Source can be Nd2O3And source of aluminium can be Al2O3, purity is more than 99.9%.
In the present invention, the binding agent is the polyvinyl alcohol that concentration is 6%~8%, the binding agent and the preburning powdered material
Mass ratio is (0.06~0.08):1.
Method of the present invention preparation process is simple, process is pollution-free, and repeatability is good, and obtained medium dielectric constant microwave medium microwave is situated between
Ceramics microwave dielectric property is excellent, has broad application prospects.
Brief description of the drawings
Fig. 1 is the ESEM scanning figure of intermediary's microwave-medium ceramics prepared by embodiment 1.
Specific embodiment
With reference to the accompanying drawings, by specific embodiment, the invention will be further described, to more fully understand the present invention.
It is an object of the present invention to provide a kind of process is simple and the microwave dielectric ceramic with medium dielectric constant and its system of stable performance
Preparation Method.Microwave-medium ceramics of the invention, preparation process is simple, repeatability is good, and microwave dielectric property is excellent.
The microwave dielectric ceramic with medium dielectric constant that the present invention is provided, its raw material composition is Nd0.34Ca0.396Sr0.264Al0.34Ti0.66O3。
The microwave dielectric ceramic with medium dielectric constant has a positive temperature coefficient of resonance frequency (1~3ppm/ DEG C), Medium dielectric constant (42~
43), high quality factor (Q × f is 30000~40000GHz).
CaCO can be used as above-mentioned ceramic material is prepared3、SrCO3、TiO2、Nd2O3And Al2O3As raw material.Ying Li
Solution, these raw materials be only it is preferred, also can using others can generate corresponding element oxide as calcium source, barium source, titanium source,
Neodymium source and silicon source.The purity of raw material is preferably more than 99.9%.
Above-mentioned chemical raw material (calcium source, barium source, titanium source, neodymium source and silicon source) is pressed into Nd respectively0.34Ca0.396Sr0.264Al0.34Ti0.66O3
Stoichiometric proportion weighs dispensing, and being put into ball grinder carries out a ball milling, and then drying and screening, can obtain original powder；Ball
Mill can be using zirconia ball and deionized water as abrading-ball and ball-milling medium, and the mass ratio of powder, zirconia ball and deionized water can
It is 1:2:2, Ball-milling Time can be 12~24 hours.To be dried in raw material after ball milling and drying box, sieving, wherein, sieving
Aperture be 20 mesh.
By gained original powder at 1350 DEG C~1450 DEG C after pre-burning 4~6 hours, being put into ball grinder carries out secondary ball milling,
Then drying can obtain preburning powdered material.
As binding agent and granulated to the polyvinyl alcohol for adding concentration to be 6%~8% in preburning powdered material, the binding agent with it is described
The mass ratio of preburning powdered material is (0.06~0.08):1, it is pressed into cylindric idiosome.The blank shape of compacting can be but be not limited to justify
Column, can be adjusted according to actual needs.
Gained idiosome is being sintered 4~12 hours at 1450~1550 DEG C, that is, is obtaining described intermediary's microwave-medium ceramics.
Embodiment is enumerated further below to describe the present invention in detail.It will similarly be understood that following examples are served only for the present invention
It is further described, it is impossible to be interpreted as limiting the scope of the invention, on those skilled in the art is of the invention
State some nonessential modifications and adaptations that content makes and belong to protection scope of the present invention.Following specific technological parameters of example
Deng being also only an example in OK range, i.e. those skilled in the art can be done in suitable scope by the explanation of this paper and be selected
Select, and do not really want to be defined in the concrete numerical value of hereafter example.
Embodiment 1
The present invention is more than 99.9%CaCO using purity3、SrCO3、TiO2、Nd2O3And Al2O3As preparation
Nd0.34Ca0.396Sr0.264Al0.34Ti0.66O3Microwave-medium ceramics, specific embodiment is as follows：
1) CaCO that purity is 99.9% is weighed respectively3、SrCO3、TiO2、Nd2O3 and Al2O3Respectively in molar ratio
2.38gCaCO3、2.18gSrCO3、3.18gTiO2、3.45gNd2O3And 1.05gAl2O3, nylon is added raw materials into after mixing
In tank, 25 grams of zirconia balls and 25ml deionized waters, ball milling, drying, sieving are added；
2) 1) gained powder is calcined 4 hours at 1350 DEG C~1450 DEG C, the powder after calcining is placed again into be added in ball grinder
25g zirconia balls and 25g deionized waters, secondary ball milling 6 hours, drying；
3) to 2) to adding weight/mass percentage composition to be polyvinyl alcohol that 8% concentration is 6% as binding agent and granulate in the powder of drying,
Cylindric idiosome is pressed into, cylindric idiosome is incubated 4 hours at 1450 DEG C sinters porcelain into, that is, obtains required middle dielectric microwave
Media ceramic.
Embodiment 2
Embodiment 1 is repeated, but the sintered heat insulating time is 6 hours.
Embodiment 3
Embodiment 1 is repeated, but the secondary ball milling time is 8 hours, and the sintered heat insulating time is 12 hours.
Embodiment 4
Embodiment 1 is repeated, but a Ball-milling Time is 18 hours, and the secondary ball milling time is 8 hours, and sintering temperature is 1500 DEG C, is burnt
Knot soaking time is 4 hours.
Embodiment 5
Embodiment 1 is repeated, but a Ball-milling Time is 18 hours, and the secondary ball milling time is 10 hours, and sintering temperature is 1500 DEG C,
The sintered heat insulating time is 6 hours.
Embodiment 6
Embodiment 1 is repeated, but a Ball-milling Time is 18 hours, and the secondary ball milling time is 10 hours, and sintering temperature is 1500 DEG C,
The sintered heat insulating time is 12 hours.
Embodiment 7
Embodiment 1 is repeated, but a Ball-milling Time is 20 hours, and the secondary ball milling time is 11 hours, and sintering temperature is 1550 DEG C,
The sintered heat insulating time is 4 hours.
Embodiment 8
Embodiment 1 is repeated, but a Ball-milling Time is 22 hours, and the secondary ball milling time is 11 hours, and sintering temperature is 1550 DEG C,
The sintered heat insulating time is 6 hours.
Embodiment 9
Embodiment 1 is repeated, but a Ball-milling Time is 24 hours, and the secondary ball milling time is 12 hours, and sintering temperature is 1550 DEG C,
The sintered heat insulating time is 12 hours.
The microwave dielectric property of intermediary's microwave-medium ceramics obtained in above-described embodiment is tested with tester (Network Analyzer),
Its test result refers to table 1.
Table 1
By Agilent E8363A PNA Network Analyzers, using the prepared cylindrical ceramic material of open type parallel plate method measurement
Dielectric constant, test furniture is put into ESPEC MC-710F type high/low temperature circulating boxes and carries out the survey of temperature coefficient of resonance frequency
Amount, temperature range is 20~80 DEG C of test frequencies in the range of 4.2~4.5GHz.
Using the quality factor of the prepared cylindrical ceramic sample of enclosed cell method measurement, test frequency is in the range of 9~10GHz.
Claims (6)
1. a kind of middle-dielectric constant microwave-medium ceramic material, it is characterised in that the chemical formula of the ceramic material is Nd0.34Ca0.396Sr0.264Al0.34Ti0.66O3。
2. according to claim 1 intermediary microwave dielectric ceramic materials, it is characterised in that the dielectric constant of the ceramic material is 42~43.
3. according to the intermediary's microwave dielectric ceramic materials of claim 1 or 2, it is characterised in that the quality factor q × f of the ceramic material is 30000~40000GHz.
4. the preparation method of the middle-dielectric constant microwave-medium ceramic material any one of a kind of claim 1-3, it is characterised in that the preparation method includes：
（1）Chemical raw material calcium source, barium source, titanium source, neodymium source and silicon source are weighed into dispensing by the chemical formula respectively, ball milling drying and screening after 12~24 hours obtains original powder；
（2）By gained original powder at 1350 DEG C~1450 DEG C after pre-burning 4~6 hours, secondary ball milling 6~12 hours, drying obtains preburning powdered material；
（3）To adding binding agent in gained preburning powdered material and granulating, idiosome is pressed into；
（4）Gained idiosome is sintered 4~12 hours at 1450~1550 DEG C, described intermediary's microwave dielectric ceramic materials are obtained.
5. preparation method according to claim 4, it is characterised in that the calcium source is CaCO3, the barium source be SrCO3, the titanium source be TiO2, the neodymium source be Nd2O3And source of aluminium is Al2O3, purity is more than 99.9%.
6. the preparation method according to claim 4 or 5, it is characterised in that the binding agent is the polyvinyl alcohol that concentration is 6%~8%, and the binding agent is with the mass ratio of the preburning powdered material（0.06~0.08）：1.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103360050A (en) * | 2013-07-11 | 2013-10-23 | 华中科技大学 | Medium-dielectric-constant microwave dielectric ceramic and preparation method thereof |
| CN103482978A (en) * | 2012-10-30 | 2014-01-01 | 清华大学 | Solid-solution microwave dielectric ceramic material, and preparation method and application 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 |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103482978A (en) * | 2012-10-30 | 2014-01-01 | 清华大学 | Solid-solution microwave dielectric ceramic material, and preparation method and application thereof |
| CN103360050A (en) * | 2013-07-11 | 2013-10-23 | 华中科技大学 | Medium-dielectric-constant microwave dielectric ceramic 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 |
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Application publication date: 20170707 |