CN108249917A - Microwave-medium ceramics, preparation method and applications with medium dielectric constant microwave medium and ultralow dielectric loss - Google Patents
Microwave-medium ceramics, preparation method and applications with medium dielectric constant microwave medium and ultralow dielectric loss Download PDFInfo
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Abstract
The invention discloses a kind of microwave-medium ceramics, preparation method and applications with medium dielectric constant microwave medium and ultralow dielectric loss.The chemical expression of microwave-medium ceramics of the present invention is：Sr2(Ti1‑ xZrx)O4, wherein 0<x<0.1, which is：By SrCO3、TiO2And ZrO2By the stoichiometric ratio dispensing in chemical expression, continuous ball milling is dried afterwards for 24 hours, sieving；By powder obtained after 1200 DEG C~1250 DEG C are calcined 1~3 hour, secondary ball milling is simultaneously sieved；By powder pressing obtained into green compact, 1~3 hour obtained ceramic block is sintered at 1475 DEG C~1550 DEG C.Invent the Sr prepared2(Ti0.975Zr0.025)O4Excellent ε in ceramicsrIt is far superior to other microwave dielectric material systems with Qf value combining properties, can be widely applied in wireless telecommunications system such as microwave resonator, microwave filter component, have great application value in fields such as base station communication, satellite communications.
Description
Technical field
The invention belongs to technical field of ceramic material, have medium dielectric constant microwave medium and ultralow dielectric loss more particularly to one kind
Microwave-medium ceramics, preparation method and applications.
Background technology
Microwave-medium ceramics refer to be applied to be used as dielectric material in microwave frequency band (300MHz-300GHz) circuit and complete
The low-loss of one or more functions, temperature-stable ceramics.With the fast development of wireless communication technique, microwave-medium ceramics
Critical material as passive devices such as microwave resonance device (including dielectric resonator, wave filter, oscillator), microwave capacitors
And it gets the attention.In order to meet device miniaturization and practical demand, while cost is taken into account, it is desirable that this kind of ceramics
With larger dielectric constant (εr), relatively low dielectric loss (i.e. higher Qf values) and good temperature stability.In recent years,
With continuous improvement of the people to requirements such as transinformation content, speed and quality, generation information transmission technology such as 5G movements
Communication, Internet of Things (IoT) technology etc. continue to bring out.To meet the application demand of following mechanics of communication, there is an urgent need for excavate to have medium
The performance boundary of material and exploration novel microwave dielectric material system.
It is theoretical by dielectric it is found that dielectric constant and the Qf values of material typically exhibit negative correlativing relation, i.e. dielectric constant
The decline for being usually associated with Qf values is improved, thus there is the material system of larger dielectric constant and ultralow dielectric loss simultaneously very
Lack.On the other hand, although microwave current media ceramic has obtained extensive research, a series of new microwave dielectric material is not yet
It is disconnected to emerge in large numbers, but with medium dielectric constant microwave medium (40<εr<70) ceramics as low-loss microwave medium system is but almost blank.Patent
Applicant is in Sr2TiO4Find that it has very excellent ε r and Qf value combining properties (ε in ceramicsr=42, Qf=
145200GHz), and Paper Writing is published in (S on the authority's SCI periodicals of dielectric fieldrn+1TinO3n+1(n=1,2)
Microwave Dielectric Ceramics with Medium Dielectric Constant and Ultra-Low
Dielectric Loss,"J.Am.Ceram.Soc.,2017,100,496-500).Further, due to ceramic microwave dielectric
The factors such as performance and material structure, micro-structure are closely related and dielectric loss is originating primarily from ceramic internal flaw such as crystal boundary, gas
The micro-structures factor such as hole, the possibility for then containing ceramic microwave dielectric properties by optimizing micro-structure and further improving.For this purpose, this
Invention is around Sr2TiO4Ceramic B ion modification regulates and controls its micro-structure and microwave dielectric property, develops a kind of with dielectric
Microwave-medium ceramics of constant and ultralow dielectric loss and preparation method thereof, the results showed that：Micro Zr ion exchanges Ti ion energy
Effectively regulate and control Sr2TiO4The crystallite dimension and microscopic appearance of ceramics, so as in Sr2(Ti1-xZrx)O4Microwave is obtained in material to be situated between
Electrical property is further promoted.
Invention content
First of the present invention is designed to provide a kind of microwave-medium with medium dielectric constant microwave medium and ultralow dielectric loss
Ceramics.Sr prepared by the present invention2(Ti1-xZrx)O4Permittivity ε of the ceramics under microwave frequency bandrIt is for 38.7~42.6, Qf values
35700~160000GHz has great application value in fields such as base station communication, satellite communications.
Another object of the present invention is to provide the preparation method of above-mentioned microwave-medium ceramics.
It is still another object of the present invention to provide the applications of above-mentioned microwave-medium ceramics.
To achieve the above object, the present invention takes following technical scheme：
A kind of microwave-medium ceramics with medium dielectric constant microwave medium and ultralow dielectric loss, microwave-medium ceramics chemistry expression
Formula is：Sr2(Ti1-xZrx)O4, wherein 0≤x≤0.1, the ceramics are under microwave frequency band, permittivity εrIt is 38.7~42.6,
Qf values are 35700~160000GHz when test frequency is 6GHz.
A kind of preparation method of the microwave-medium ceramics with medium dielectric constant microwave medium and ultralow dielectric loss, including walking as follows
Suddenly：
(1) by SrCO3、TiO2And ZrO2By the stoichiometric ratio dispensing in chemical expression, continuous ball milling is dried afterwards for 24 hours,
Sieving；
(2) by powder made from step (1) after 1200 DEG C~1250 DEG C are calcined 1-3 hours, secondary ball milling is simultaneously sieved；
(3) into green compact ceramics are made in 1-3 hours in 1475 DEG C~1550 DEG C sintering in powder pressing made from step (2)
Block.
The present invention is in Sr2TiO4By controlling the content of Zr ion exchange Ti ions and being controlled in sintering process in ceramics
Powder forming core processed is grown up degree, so as to influence crystallite dimension and microscopic appearance in ceramic microstructures, finally realizes microwave dielectric property
Improved purpose can be regulated and controled.
Before preparation, raw material needs to be ground to certain fineness, during grinding, raw material can be put into ball grinder, add in oxidation
Zirconium ball-milling medium and absolute ethyl alcohol continuous ball milling 24 hours or more.
Further, in step (1), SrCO is selected3、TiO2And ZrO2Purity >=99.99%.
Further, in step (2), calcination temperature is 1225 DEG C.
Further, in step (3), the sintering atmosphere of green compact is air environment, and heating rate is 5 DEG C/min, has been sintered
1100 DEG C and then furnace cooling are cooled to the speed control of 2 DEG C/min after.
A kind of application of microwave-medium ceramics with medium dielectric constant microwave medium and ultralow dielectric loss in the field of communications.
Compared with prior art, the beneficial effects of the present invention are：
Sr prepared by the present invention2(Ti0.975Zr0.025)O4Ceramics only need by micro Zr ionic portions replace Ti from
Son just can obtain extremely excellent microwave dielectric property (εr=42.6, Qf=160000GHz).Applicant is analogous to before to exist
Sr reported in the literature2TiO4Microwave dielectric property (the ε of ceramicsr=42, Qf=145200GHz), dielectric constant improves 0.6,
Qf values improve 14800GHz.In addition, Sr prepared by the present invention2(Ti0.975Zr0.025)O4Excellent ε in ceramicsrWith Qf value performances
Combination is far superior to other microwave dielectric material systems, can be widely applied to wireless telecommunications system such as microwave resonator, microwave and filters
In the components such as wave device, there is great application value in fields such as base station communication, satellite communications.
Description of the drawings
Fig. 1 is Sr2(Ti1-xZrx)O4Ceramic powders XRD diffracting spectrums：(a) x=0 (comparative example 1), (b) x=0.025 are (real
Apply example 1), (c) x=0.05 (embodiment 2), (d) x=0.10 (embodiment 3)；
Fig. 2 is Sr2(Ti1-xZrx)O4The sintered surface of ceramics and break surface SEM image：(a), (b) x=0 (comparative examples
1)；(c), (d) x=0.025 (embodiment 1)；(e), (f) x=0.05 (embodiment 2)；(h), (i) x=0.10 (embodiment 3)；
Fig. 3 is Sr2(Ti1-xZrx)O4(x=0.0,0.025,0.05,0.10) ceramics εrWith the variation diagram of sintering temperature；
Fig. 4 is Sr2(Ti1-xZrx)O4(x=0.0,0.025,0.05,0.10) ceramics Qf values with sintering temperature variation diagram.
Specific embodiment
Specific examples below is the further explanation to method provided by the invention and technical solution, but is not construed as
Limitation of the present invention.
Embodiment 1
(1) by SrCO3、TiO2And ZrO2Raw material powder (purity 99.99%) presses Sr respectively2(Ti0.975Zr0.025)O4Chemistry
Metering is than weighing dispensing；
(2) step (1) prepared chemical raw material is put into ball grinder, adds in zirconia ball and absolute ethyl alcohol ball milling 24 is small
When, 120 mesh sieve is crossed after the powder after ball milling is dried in drying box；
(3) secondary ball milling is carried out after powder made from step (2) is calcined 3 hours at 1225 DEG C, 120 mesh are crossed after drying
Sieve；
(4) PVA solution of 4wt% is added in powder made from step (3) and is ground uniformly, crosses 40 mesh sieve；Then, will
Gained powder is put into the stainless steel mould of a diameter of 12mm, the pressurize 5min under 98MPa pressure, obtains the pottery that thickness is 5mm
Porcelain green compact.Gained ceramic green is sintered 3h at 1475 DEG C -1550 DEG C and finally obtains ceramics sample.The heating speed of sintering process
It spends for 5 DEG C/min, program is controlled to be down to 1100 DEG C with the speed of 2 DEG C/min after sintering, then furnace cooling to room temperature, obtains
The XRD diagram of the microwave-medium ceramics arrived is referring to Fig. 1.
Embodiment 2
(1) by SrCO3、TiO2And ZrO2Raw material powder (purity 99.99%) presses Sr respectively2(Ti0.95Zr0.05)O4Chemistry meter
Amount is than weighing dispensing；
(2) step (1) prepared chemical raw material is put into ball grinder, adds in zirconia ball and absolute ethyl alcohol ball milling 24 is small
When, 120 mesh sieve is crossed after the powder after ball milling is dried in drying box；
(3) secondary ball milling is carried out after powder made from step (2) is calcined 3 hours at 1250 DEG C, 120 mesh are crossed after drying
Sieve；
(4) PVA solution of 4wt% is added in powder made from step (3) and is ground uniformly, crosses 40 mesh sieve；Then, will
Gained powder is put into the stainless steel mould of a diameter of 12mm, the pressurize 5min under 98MPa pressure, obtains the pottery that thickness is 5mm
Porcelain green compact.Gained ceramic green is sintered 3h at 1475 DEG C -1550 DEG C and finally obtains ceramics sample.The heating speed of sintering process
It spends for 5 DEG C/min, program is controlled to be down to 1100 DEG C with the speed of 2 DEG C/min after sintering, then furnace cooling to room temperature, obtains
The XRD diagram of the microwave-medium ceramics arrived is referring to Fig. 1.
Embodiment 3
(1) by SrCO3、TiO2And ZrO2Raw material powder (purity 99.99%) presses Sr respectively2(Ti0.9Zr0.1)O4Stoichiometry
Than weighing dispensing；
(2) step (1) prepared chemical raw material is put into ball grinder, adds in zirconia ball and absolute ethyl alcohol ball milling 24 is small
When, 120 mesh sieve is crossed after the powder after ball milling is dried in drying box；
(3) secondary ball milling is carried out after powder made from step (2) is calcined 3 hours at 1250 DEG C, 120 mesh are crossed after drying
Sieve；
(4) PVA solution of 4wt% is added in powder made from step (3) and is ground uniformly, crosses 40 mesh sieve；Then, will
Gained powder is put into the stainless steel mould of a diameter of 12mm, the pressurize 5min under 98MPa pressure, obtains the pottery that thickness is 5mm
Porcelain green compact.Gained ceramic green is sintered 3h at 1475 DEG C -1550 DEG C and finally obtains ceramics sample.The heating speed of sintering process
It spends for 5 DEG C/min, program is controlled to be down to 1100 DEG C with the speed of 2 DEG C/min after sintering, then furnace cooling to room temperature, obtains
The XRD diagram of the microwave-medium ceramics arrived is referring to Fig. 1.
Comparative example 1
(1) by SrCO3And TiO2Raw material powder (purity 99.99%) presses Sr respectively2TiO4Stoichiometric ratio weighs dispensing；
(2) step (1) prepared chemical raw material is put into ball grinder, adds in zirconia ball and absolute ethyl alcohol ball milling 24 is small
When, 120 mesh sieve is crossed after the powder after ball milling is dried in drying box；
(3) secondary ball milling is carried out after powder made from step (2) is calcined 3 hours at 1200 DEG C, 120 mesh are crossed after drying
Sieve；
(4) PVA solution of 4wt% is added in powder made from step (3) and is ground uniformly, crosses 40 mesh sieve；Then, will
Gained powder is put into the stainless steel mould of a diameter of 12mm, the pressurize 5min under 98MPa pressure, obtains the pottery that thickness is 5mm
Porcelain green compact.Gained ceramic green is sintered 3h at 1475 DEG C -1550 DEG C and finally obtains ceramics sample.The heating speed of sintering process
It spends for 5 DEG C/min, program is controlled to be down to 1100 DEG C with the speed of 2 DEG C/min after sintering, then furnace cooling to room temperature, obtains
The XRD diagram of the microwave-medium ceramics arrived is referring to Fig. 1.
Scanning electron is used after the cylindrical dielectric ceramic surface that Examples 1 to 3 and comparative example 1 are prepared is sprayed gold
Micro- sem observation sample surfaces and section crystallite dimension and microscopic appearance, referring to Fig. 2.Using abrasive paper for metallograph to sample after observation
Product surface carries out grinding-polishing, until naked eyes are not it is observed that apparent cut.Network analysis is used after sample ultrasonic concussion cleaning
Instrument distinguishes the dielectric constant of test sample and Qf values, gained performance with the figure that sintering temperature changes referring to Fig. 3,4.
Table 1
Table 1, which is shown, utilizes Sr made from the preparation method of the present invention2TiO4(comparative example) and Sr2(Ti1-xZrx)O4(implement
Example) ceramics optimal εrWith Qf values.
As shown in Table 1, in Sr2TiO4Its micro-wave dielectric can be significantly affected by Zr ion exchange Ti ions in ceramics
Performance, and Sr2(Ti0.975Zr0.025)O4Ingredient dielectric properties are substantially better than pure Sr in comparative example2TiO4Ceramics, optimal εrFor
42.6, optimal Qf values are 160000GHz.
The explanation of above example is only intended to help to understand the method for the present invention and its core concept.It should be pointed out that for
For those skilled in the art, without departing from the principle of the present invention, if can also be carried out to the present invention
Dry improvement and modification, these improvement and modification are also fallen into the claims in the present invention protection domain.
Claims (8)
1. a kind of microwave-medium ceramics with medium dielectric constant microwave medium and ultralow dielectric loss, which is characterized in that the microwave-medium is made pottery
Porcelain chemical expression is：Sr2(Ti1-xZrx)O4, wherein 0<x<0.1, the ceramics are under microwave frequency band, permittivity εrFor
38.7~42.6, Qf value are 35700~160000GHz when test frequency is 6GHz.
2. a kind of preparation side of microwave-medium ceramics with medium dielectric constant microwave medium and ultralow dielectric loss as described in claim 1
Method includes the following steps：
(1) by raw material SrCO3、TiO2And ZrO2By the stoichiometric ratio dispensing in chemical expression, continuous ball milling is dried afterwards for 24 hours,
Sieving；
(2) by powder made from step (1) after 1200 DEG C~1250 DEG C are calcined 1~3 hour, secondary ball milling is simultaneously sieved；
(3) powder pressing made from step (2) is sintered 1~3 hour obtained ceramic block into green compact at 1475 DEG C~1550 DEG C
Body.
3. preparation method as claimed in claim 2, which is characterized in that before preparation, raw material needs are fully ground and cross 120 mesh
Sieve.
4. preparation method as claimed in claim 2, which is characterized in that the ball grinder adds in zirconium oxide ball milling and secondary ball
Mill is in ball grinder, adds in zirconia ball and absolute ethyl alcohol continuous ball milling 24 hours or more.
5. preparation method as claimed in claim 2, which is characterized in that SrCO3、TiO2And ZrO2Purity >=99.99%.
6. preparation method as claimed in claim 2, which is characterized in that in the step (2), calcination temperature is 1225 DEG C.
7. preparation method as claimed in claim 2, which is characterized in that in step (3), the sintering atmosphere of green compact is air ring
Border, heating rate are 5 DEG C/min, and 1100 DEG C and then furnace cooling are cooled to the speed control of 2 DEG C/min after the completion of sintering.
What 8. any one of microwave-medium ceramics as described in claim 1 or claim 2-7 preparation method were prepared
The application of microwave-medium ceramics in the field of communications.
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| CN113072373A (en) * | 2021-04-12 | 2021-07-06 | 合肥工业大学 | Temperature-stable low-dielectric ceramic material suitable for 5G millimeter wave communication application and preparation method thereof |
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| CN113072373A (en) * | 2021-04-12 | 2021-07-06 | 合肥工业大学 | Temperature-stable low-dielectric ceramic material suitable for 5G millimeter wave communication application and preparation method thereof |
| CN113149628A (en) * | 2021-04-22 | 2021-07-23 | 安徽沃信通信科技有限公司 | Microwave ceramic dielectric material capable of improving anti-reduction capability and preparation method thereof |
| CN113149628B (en) * | 2021-04-22 | 2022-09-13 | 安徽沃信通信科技有限公司 | Microwave ceramic dielectric material capable of improving anti-reduction capability and preparation method thereof |
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