CN107311646A - A kind of preparation method for improving strontium titanate ceramicses dielectric material performance - Google Patents

A kind of preparation method for improving strontium titanate ceramicses dielectric material performance Download PDF

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CN107311646A
CN107311646A CN201710465714.3A CN201710465714A CN107311646A CN 107311646 A CN107311646 A CN 107311646A CN 201710465714 A CN201710465714 A CN 201710465714A CN 107311646 A CN107311646 A CN 107311646A
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strontium titanate
preparation
powder
dielectric material
ball
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李玲霞
陈思亮
于仕辉
郑浩然
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Tianjin University
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Tianjin University
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    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/46Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
    • C04B35/462Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates
    • C04B35/465Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates
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Abstract

, first will be by raw material SrCO the invention discloses a kind of preparation method for improving strontium titanate ceramicses dielectric material performance3、TiO2、Al2O3、Nb2O5By SrTi1‑x(Al0.5Nb0.5)xO3Wherein the chemical formula of x=0.03~0.15 weighs dispensing, again after ball milling, drying, sieving, in being calcined at 1150 DEG C, principal crystalline phase is synthesized, then after granulation, it is compressing for base substrate with 3MPa pressure, base substrate is incubated 4 hours, the strontium titanate ceramicses material with low-dielectric loss, low resonant frequency temperature coefficient is made in 1350~1450 DEG C of sintering.Ceramic dielectric constant ε of the present inventionrFor 72.4~274.0, quality factor q f values are 2946.5GHz~9077.0GHz, temperature coefficient of capacitance τf587 × 10‑6/ DEG C~1325 × 10‑6/ DEG C in the range of.This method has been obviously improved the quality factor of material, while reducing τfValue.

Description

A kind of preparation method for improving strontium titanate ceramicses dielectric material performance
Technical field
The invention belongs to a kind of ceramic composition being characterized with composition, more particularly to one kind is with SrTi1-x (Al0.5Nb0.5)xO3For chemical formula, improve product Qf values and reduce τfPreparation method.
Background technology
In recent years, demand day of the sustainable development of mobile communication to microwave devices such as resonator, wave filter, diectric antennas Benefit increases, while proposing higher requirement to its performance.As the microwave-medium ceramics of these component critical materials, especially It is the concern of the microwave-medium ceramics of high-k, extremely various countries researcher.
It is mainly normal with higher dielectric towards exploring since microwave dielectric ceramic materials produce differentiation from 1990s Number (εr>100) new system is carried out with ultra-low loss (especially medium dielectric constant microwave medium class) two important directions are pursued.Due to The square root of the size and dielectric constant of resonator and wave filter is inversely proportional, and the microwave-medium ceramics of high-k are logical in microwave The application in circuit is interrogated, microwave telecommunication devices will be greatly facilitated fast-developing to miniaturization, integrated direction.
The content of the invention
The purpose of the present invention, is to improve SrTiO in order to further on the basis of existing technology3The Qf values of ceramic material are simultaneously Reduce τfValue, to adapt to electronic information technology high frequency and digitized developing direction.With SrCO3、TiO2、Al2O3、Nb2O5For Raw material, is prepared a kind of with the low τ of high quality factor by simple solid phase methodfThe microwave dielectric ceramic materials of value.
The present invention is achieved by following technical solution.
A kind of preparation method for improving strontium titanate ceramicses dielectric material performance, specific implementation step is as follows:
(1) by raw material SrCO3、TiO2、Al2O3、Nb2O5By SrTi1-x(Al0.5Nb0.5)xO3, wherein x=0.03~0.15 Chemical formula weighs dispensing;
(2) powder for preparing step (1) is put into ball grinder, adds zirconia ball and absolute ethyl alcohol, ball milling 6 hours; Raw material after ball milling is placed in infrared drying oven and dried, 40 mesh sieves are crossed after drying, evengranular powder is obtained;
(3) powder after step (2) processing is synthesized into principal crystalline phase in being calcined 4 hours at 1150 DEG C;
(4) polyvinyl alcohol that additional mass percent is 0.75% in the powder after step (3) processing, is put into ball grinder In, zirconia ball and absolute ethyl alcohol are added, ball milling 12 hours crosses 80 mesh sieves after drying, then with powder compressing machine with 3MPa pressure Compressing power is base substrate;
(5) base substrate after step (4) is molded is incubated 4 hours, is made and is damaged with low dielectric in 1350~1450 DEG C of sintering Consumption, the strontium titanate ceramicses material of low resonant frequency temperature coefficient.
The drying temperature of the step (2) and step (4) is 100 DEG C.
The mass ratio of the ceramic powder of the step (2) and step (4) and zirconia ball, deionized water is 1:1:2.
The base substrate of the step (4) is Φ 10mm × 5mm disk.
The sintering temperature of the step (5) is 1400 DEG C.
Beneficial effects of the present invention, there is provided a kind of high-k, low-dielectric loss, low resonant frequency temperature coefficient Material and preparation method thereof, obtained SrTi1-x(Al0.5Nb0.5)xO3(x=0.03,0.05,0.1,0.15) material dielectric constant εrFor 72.4~274.0, quality factor q f values are 2946.5GHz~9077.0GHz, temperature coefficient of capacitance τf587 × 10-6/ DEG C~1325 × 10-6/ DEG C in the range of.This method has been obviously improved the quality factor of material, while reducing τfValue.
Embodiment
The present invention is with SrCO3(analysis is pure), Nb2O5(analysis is pure), Al2O3(analysis is pure), TiO2(analysis is pure) is initial former Material, microwave-medium ceramics are prepared by simple solid-phase synthesis.Specific embodiment is as follows:
Embodiment 1
1. by raw material SrCO3、TiO2、Al2O3、Nb2O5Stoichiometrically formula SrTi0.9(Al0.5Nb0.5)0.1O3Weigh dispensing, Powder is matched:12.9085g SrCO3、6.2876g TiO2、0.2229g Al2O3、0.5811g Nb2O5.By the mixed of about 20g Close powder to be put into nylon tank, add 200ml absolute ethyl alcohols, after the zirconium ball for adding 150g, ball milling 6 is small on planetary ball mill When, rotating speed is 400 revs/min;
2. the raw material after ball milling is placed in drying box, 40 mesh sieves are crossed after being dried in 100 DEG C;
3. the powder after drying sieving is put into moderate oven, in 1150 DEG C of pre-burnings, 4 hours are incubated;
4. the polyvinyl alcohol that 0.75% is added in the powder after step 3 pre-burning is mixed as adhesive, ball is put into In grinding jar, add zirconia ball and/or absolute ethyl alcohol, ball milling 12 hours crosses 80 mesh sieves after drying, then with powder compressing machine with 3MPa pressure is pressed into base substrate;
5. base substrate is incubated 4 hours, the strontium titanates microwave-medium ceramics material of high dielectric property is made in 1400 DEG C of sintering Material.
6. the microwave property of resulting product is tested by Network Analyzer.
Embodiment 2~12
The preparation method of specific embodiment 2~12 is substantially the same manner as Example 1, its main technologic parameters and its micro-wave dielectric Performance refers to table 1.
Table 1
The present invention is not limited to above-described embodiment, and the change of some details is possible, but therefore this do not run counter to this hair Bright scope and spirit.

Claims (5)

1. a kind of preparation method for improving strontium titanate ceramicses dielectric material performance, specific implementation step is as follows:
(1) by raw material SrCO3、TiO2、Al2O3、Nb2O5By SrTi1-x(Al0.5Nb0.5)xO3, the wherein chemistry of x=0.03~0.15 Formula weighs dispensing;
(2) powder for preparing step (1) is put into ball grinder, adds zirconia ball and absolute ethyl alcohol, ball milling 6 hours;By ball Raw material after mill is placed in infrared drying oven and dried, and 40 mesh sieves are crossed after drying, obtains evengranular powder;
(3) powder after step (2) processing is synthesized into principal crystalline phase in being calcined 4 hours at 1150 DEG C;
(4) polyvinyl alcohol that additional mass percent is 0.75% in the powder after step (3) processing, is put into ball grinder, Zirconia ball and absolute ethyl alcohol are added, ball milling 12 hours crosses 80 mesh sieves after drying, then with powder compressing machine with 3MPa pressure pressure System is shaped to base substrate;
(5) by step (4) be molded after base substrate in 1350~1450 DEG C sintering, be incubated 4 hours, be made with low-dielectric loss, The strontium titanate ceramicses material of low resonant frequency temperature coefficient;
2. a kind of preparation method for improving strontium titanate ceramicses dielectric material performance according to claim 1, it is characterised in that The drying temperature of the step (2) and step (4) is 100 DEG C.
3. a kind of preparation method for improving strontium titanate ceramicses dielectric material performance according to claim 1, it is characterised in that The mass ratio of the ceramic powder of the step (2) and step (4) and zirconia ball, deionized water is 1:1:2.
4. a kind of preparation method for improving strontium titanate ceramicses dielectric material performance according to claim 1, it is characterised in that The base substrate of the step (4) is Φ 10mm × 5mm disk.
5. a kind of preparation method for improving strontium titanate ceramicses dielectric material performance according to claim 1, it is characterised in that The sintering temperature of the step (5) is 1400 DEG C.
CN201710465714.3A 2017-06-19 2017-06-19 A kind of preparation method for improving strontium titanate ceramicses dielectric material performance Pending CN107311646A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108178628A (en) * 2018-01-24 2018-06-19 天津大学 A kind of method for preparing low-loss huge dielectric constant medium ceramic material
CN108285344A (en) * 2018-01-17 2018-07-17 天津大学 A kind of low-loss ixiolite structure microwave dielectric ceramic materials
CN108314444A (en) * 2018-03-12 2018-07-24 天津大学 A kind of high q-factor rock salt class microwave dielectric material
CN108439973A (en) * 2018-01-17 2018-08-24 天津大学 A kind of high q-factor high-dielectric constant microwave-medium ceramics material and preparation method thereof
CN108751981A (en) * 2018-08-15 2018-11-06 天津大学 A kind of aluminium niobium is co-doped with microwave dielectric ceramic with medium dielectric constant and preparation method thereof
CN114644519A (en) * 2022-02-28 2022-06-21 华南理工大学 Dielectric ceramic material and preparation method thereof
CN114716243A (en) * 2022-04-12 2022-07-08 华南理工大学 High-temperature stable sodium bismuth titanate-strontium titanate-based dielectric energy storage ceramic material and preparation and application thereof

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CN102603282A (en) * 2012-03-22 2012-07-25 桂林理工大学 Ultralow-temperature sintering temperature stable-type microwave dielectric ceramic and preparation method thereof
CN103864426A (en) * 2014-01-21 2014-06-18 天津大学 Medium-sintering temperature stable microwave dielectric ceramic material
CN103951428A (en) * 2014-04-23 2014-07-30 天津大学 Moderate-temperature stable-sintering-temperature low-loss microwave dielectric ceramic material
CN104402437A (en) * 2014-09-19 2015-03-11 天津大学 Low-temperature sintered NdNbO4-CaTiO3 series microwave dielectric ceramic and preparation method thereof
CN105060887A (en) * 2015-07-24 2015-11-18 天津大学 Low-temperature sintering low loss microwave dielectric ceramic material

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102603282A (en) * 2012-03-22 2012-07-25 桂林理工大学 Ultralow-temperature sintering temperature stable-type microwave dielectric ceramic and preparation method thereof
CN103864426A (en) * 2014-01-21 2014-06-18 天津大学 Medium-sintering temperature stable microwave dielectric ceramic material
CN103951428A (en) * 2014-04-23 2014-07-30 天津大学 Moderate-temperature stable-sintering-temperature low-loss microwave dielectric ceramic material
CN104402437A (en) * 2014-09-19 2015-03-11 天津大学 Low-temperature sintered NdNbO4-CaTiO3 series microwave dielectric ceramic and preparation method thereof
CN105060887A (en) * 2015-07-24 2015-11-18 天津大学 Low-temperature sintering low loss microwave dielectric ceramic material

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108285344A (en) * 2018-01-17 2018-07-17 天津大学 A kind of low-loss ixiolite structure microwave dielectric ceramic materials
CN108439973A (en) * 2018-01-17 2018-08-24 天津大学 A kind of high q-factor high-dielectric constant microwave-medium ceramics material and preparation method thereof
CN108178628A (en) * 2018-01-24 2018-06-19 天津大学 A kind of method for preparing low-loss huge dielectric constant medium ceramic material
CN108314444A (en) * 2018-03-12 2018-07-24 天津大学 A kind of high q-factor rock salt class microwave dielectric material
CN108751981A (en) * 2018-08-15 2018-11-06 天津大学 A kind of aluminium niobium is co-doped with microwave dielectric ceramic with medium dielectric constant and preparation method thereof
CN114644519A (en) * 2022-02-28 2022-06-21 华南理工大学 Dielectric ceramic material and preparation method thereof
CN114716243A (en) * 2022-04-12 2022-07-08 华南理工大学 High-temperature stable sodium bismuth titanate-strontium titanate-based dielectric energy storage ceramic material and preparation and application thereof

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