CN103073281A - Lithium-zinc-titanium-tin series microwave dielectric ceramics material and preparation method thereof - Google Patents
Lithium-zinc-titanium-tin series microwave dielectric ceramics material and preparation method thereof Download PDFInfo
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- CN103073281A CN103073281A CN2013100408980A CN201310040898A CN103073281A CN 103073281 A CN103073281 A CN 103073281A CN 2013100408980 A CN2013100408980 A CN 2013100408980A CN 201310040898 A CN201310040898 A CN 201310040898A CN 103073281 A CN103073281 A CN 103073281A
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Abstract
The invention discloses a lithium-zinc-titanium-tin series microwave dielectric ceramics material and a preparation method thereof. A stoichiometric equation is Li2Zn(Ti(1-x)Snx)3O8, wherein x is larger than 0 and is less than or equal to 1. The preparation method comprises the following steps of: compounding Li2CO3, ZnO, TiO2 and SnO2 according to molar ratio; carrying out ball milling; stoving; carrying out presintering at the temperature of 900 DEG C; carrying out secondary ball milling; and sintering at the temperature of 1040-1120 DEG C finally to obtain microwave dielectric ceramics. When x is equal to 0.2, a dielectric constant is 22.1, a resonant frequency temperature coefficient is -22.5ppm/DEG C, and a quality factor reaches 80500 GHz. The preparation method successfully prepares the lithium-zinc-titanium-tin series microwave dielectric ceramics for the first time, and can be applied in a crossing field of microwave dielectric ceramics and multifunctional ceramics.
Description
Technical field
The invention belongs to a kind of ceramic composition take composition as feature, particularly a kind of novel Li
2Zn (Ti
1-xSn
x)
3O
8Series microwave dielectric ceramic material and preparation method thereof.
Background technology
At present, in order to obtain practical microwave dielectric ceramic materials, need stupalith to satisfy three requirements: the DIELECTRIC CONSTANT ε that (1) is higher
r, be convenient to the miniaturization of device; (2) high quality factor (Q * f value) guarantee good selecting frequency characteristic; (3) nearly zero temperature coefficient of resonance frequency τ
f, guarantee stability.
In recent years, the researchist has studied SnO
2To Ba (Zn
1/3Nb
2/3) O
3With ZnO – TiO
2The crystalline phase of series microwave dielectric ceramic and the impact of microwave dielectric property, result of study shows SnO
2Can improve the microwave dielectric property of media ceramic.At Li
2O – ZnO – TiO
2In the three-part system, Li
2ZnTi
3O
8Pottery has good microwave dielectric property, and its microwave dielectric property is respectively ε
r=25.6, Q * f=72,000GHz, τ
f=-11.2ppm/ ° C.Yet its quality factor are still waiting to improve, and guarantee has lower loss when receiving and transmitting like this.Although the researchist is for Li
2ZnTi
3O
8Pottery carries out deep research, but to Li
2Zn (Ti
1-xSn
x)
3O
8Preparation and the microwave dielectric property of pottery yet there are no special report.The present invention adopts conventional solid-state method, prepares Novel lithium zinc titanium tin series microwave dielectric ceramic, and it has higher quality factor, and it is a kind of very promising novel microwave dielectric ceramic material.
Summary of the invention
Purpose of the present invention provides a kind of with Li
2CO
3, ZnO, TiO
2And SnO
2Be raw material, adopt conventional solid-state method to synthesize and have the Li of high quality factor
2Zn (Ti
1-xSn
x)
3O
8Series microwave dielectric ceramic, its good microwave dielectric property can be applied to the LTCC(LTCC) etc. association area.
A kind of lithium zinc titanium tin series microwave dielectric ceramic material, stoichiometric equation is Li
2Zn (Ti
1-xSn
x)
3O
8, 0＜x≤1.0 wherein;
This lithium zinc titanium tin series microwave dielectric ceramic material preparation method has following steps:
(1) be Li by stoichiometric equation
2Zn (Ti
1-xSn
x)
3O
8, 0＜x≤1.0 wherein are with raw material Li
2CO
3, ZnO, TiO
2And SnO
2It is 1:1:3 (1-x) in molar ratio: the 3x weigh batching;
(2) powder of step (1) preparation is put into ball grinder, add zirconia ball and deionized water, material, water, the mass ratio of ball are 1:7:7, ball milling 4 ~ 6 hours; Place infrared drying oven to dry the raw material behind the ball milling, cross 40 mesh sieves after the oven dry, obtain evengranular powder;
(3) powder after step (2) is processed is in 900 ℃ of lower pre-burnings 3 hours, and insulation 4 hours under this temperature, synthetic principal crystalline phase;
(4) step (3) products therefrom is put into ball grinder, in powder, adds deionized water, ball milling 4 ~ 6 hours, oven dry adds mass percent and is 6 ~ 10% paraffin and carries out granulation as tackiness agent, cross 80 mesh sieves after, be shaped to base substrate with powder compressing machine again;
(5) with the green compact after step (4) moulding in 1040 ℃ ~ 1120 ℃ sintering, be incubated 2 ~ 6 hours, make microwave-medium ceramics;
(6) microwave dielectric property of test microwave-medium ceramics.
The bake out temperature of described step (2) and step (4) is 100 ℃.
The preferred sintering temperature of described step (5) is 1080 ℃, soaking time 4h.
The base substrate of described step (4) is the right cylinder of Φ 10mm * 5mm.
The invention has the beneficial effects as follows, a kind of lithium zinc titanium tin series microwave dielectric ceramic material with good microwave dielectric property is provided, when x=0.2, quality factor reach 80500GHz., and the present invention can use the LTCC(LTCC) and the multifunctional ceramic crossing domain.
Embodiment
With Li
2CO
3, ZnO, TiO
2And SnO
2Li in molar ratio
2CO
3: ZnO:TiO
2: SnO
2=1:1:3 (1-x): x (wherein 0＜x≤1.0) weigh batching.Mixed powder is put into the polyester tank, add deionized water and zirconia ball, material, water, the mass ratio of ball is 1:7:7, and ball milling is 4 ~ 6 hours on planetary ball mill, and rotating speed is 1000 rev/mins.Again the raw material behind the ball milling is dried in the 1500W infrared drying oven, after the oven dry raw material crossed 40 mesh sieves.Powder after sieving is 900 ℃ of lower pre-burnings 3 hours, and insulation 4 hours under this temperature, synthetic principal crystalline phase.Again the powder powder after the pre-burning, add deionized water, ball milling hours 4 ~ 6 hours adds mass percent and is 8% paraffin as the tackiness agent granulation after the oven dry, cross 80 mesh sieves after, depress to the cylinder of Φ 10mm * 5mm at 4MPa pressure with powder compressing machine.Again with green compact in 1040 ~ 1120 ℃ of sintering, be incubated 2 ~ 6 hours, make microwave-medium ceramics.Pass through at last the microwave dielectric property of network analyzer test article.
Main technologic parameters and the microwave dielectric property thereof of the specific embodiment of the invention see table 1 for details.
Table 1
Claims (4)
1. lithium zinc titanium tin series microwave dielectric ceramic material, stoichiometric equation is Li
2Zn (Ti
1-xSn
x)
3O
8, 0＜x≤1 wherein;
This lithium zinc titanium tin series microwave dielectric ceramic material preparation method has following steps:
(1) be Li by stoichiometric equation
2Zn (Ti
1-xSn
x)
3O
8, 0＜x≤1 wherein is with raw material Li
2CO
3, ZnO, TiO
2And SnO
2It is 1:1:3 (1-x) in molar ratio: the 3x weigh batching;
(2) powder of step (1) preparation is put into ball grinder, add zirconia ball and deionized water, material, water, the mass ratio of ball are 1:7:7, ball milling 4 ~ 6 hours; Place infrared drying oven to dry the raw material behind the ball milling, cross 40 mesh sieves after the oven dry, obtain evengranular powder;
(3) powder after step (2) is processed is in 900 ℃ of lower pre-burnings 3 hours, and insulation 4 hours under this temperature, synthetic principal crystalline phase;
(4) step (3) products therefrom is put into ball grinder, in powder, adds deionized water, ball milling 4 ~ 6 hours, oven dry adds mass percent and is 6 ~ 10% paraffin and carries out granulation as tackiness agent, cross 80 mesh sieves after, be shaped to base substrate with powder compressing machine again;
(5) with the green compact after step (4) moulding in 1040 ℃ ~ 1120 ℃ sintering, be incubated 2 ~ 6 hours, make microwave-medium ceramics;
(6) microwave dielectric property of test microwave-medium ceramics.
2. according to claim 1 lithium zinc titanium tin series microwave dielectric ceramic material, the bake out temperature of described step (2) and step (4) is 100 ℃.
3. according to claim 1 lithium zinc titanium tin series microwave dielectric ceramic material, the preferred sintering temperature of described step (5) is 1080 ℃, soaking time 4h.
4. according to claim 1 lithium zinc titanium tin series microwave dielectric ceramic material, the base substrate of described step (4) is the right cylinder of Φ 10mm * 5mm.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104341148A (en) * | 2014-11-05 | 2015-02-11 | 天津大学 | Method for improving value Q by adopting Li2MgTi3O8-series microwave dielectric ceramics Sn4<+> to replace B-site Ti4<+> |
| CN106348756A (en) * | 2016-10-21 | 2017-01-25 | 天津大学 | High-Q-value lithium-magnesium-niobium microwave dielectric ceramic |
| CN106810209A (en) * | 2017-01-12 | 2017-06-09 | 天津大学 | A kind of high q-factor lithium magnesium titanium series microwave dielectric ceramic |
| CN106830933A (en) * | 2017-01-12 | 2017-06-13 | 天津大学 | A kind of thermally-stabilised high q-factor lithium magnesium niobium series microwave dielectric ceramic |
| CN107500753A (en) * | 2017-09-06 | 2017-12-22 | 天津大学 | A kind of low-loss titanium barium stannate dielectric material |
| CN107903059A (en) * | 2017-11-03 | 2018-04-13 | 天津大学 | A kind of intermediate sintering temperature microwave-medium ceramics and preparation method thereof |
| CN107935584A (en) * | 2017-12-12 | 2018-04-20 | 湖南先导电子陶瓷科技产业园发展有限公司 | A kind of microwave dielectric ceramic materials for LTCC and preparation method thereof |
| CN108610040A (en) * | 2018-04-27 | 2018-10-02 | 天津大学 | A method of reducing titanium barium stannate system dielectric loss under reducing atmosphere |
| CN108610041A (en) * | 2018-04-27 | 2018-10-02 | 天津大学 | A method of improving titanium barium stannate dielectric properties under reducing atmosphere |
| CN108727022A (en) * | 2018-07-04 | 2018-11-02 | 电子科技大学 | A kind of ultra-low loss magnesium-niobate lithium system microwave dielectric ceramic materials 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 |
| CN110655402A (en) * | 2019-10-14 | 2020-01-07 | 天津大学 | Medium-temperature sintered rutile-like microwave dielectric ceramic material |
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| CN102093044A (en) * | 2011-01-13 | 2011-06-15 | 天津大学 | Low-loss microwave dielectric ceramic and preparation method thereof |
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2013
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| CN102093044A (en) * | 2011-01-13 | 2011-06-15 | 天津大学 | Low-loss microwave dielectric ceramic and preparation method thereof |
Non-Patent Citations (2)
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|---|
| G.G. YAO ,P. LIU: "Effects of LiF addition on sintering behavior and microwave dielectric properties of (Mg0.95Zn0.05)2(Ti0.8Sn0.2)O4 ceramics", 《CERAMICS INTERNATIONAL》 * |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104341148A (en) * | 2014-11-05 | 2015-02-11 | 天津大学 | Method for improving value Q by adopting Li2MgTi3O8-series microwave dielectric ceramics Sn4<+> to replace B-site Ti4<+> |
| CN106348756A (en) * | 2016-10-21 | 2017-01-25 | 天津大学 | High-Q-value lithium-magnesium-niobium microwave dielectric ceramic |
| CN106810209A (en) * | 2017-01-12 | 2017-06-09 | 天津大学 | A kind of high q-factor lithium magnesium titanium series microwave dielectric ceramic |
| CN106830933A (en) * | 2017-01-12 | 2017-06-13 | 天津大学 | A kind of thermally-stabilised high q-factor lithium magnesium niobium series microwave dielectric ceramic |
| CN107500753A (en) * | 2017-09-06 | 2017-12-22 | 天津大学 | A kind of low-loss titanium barium stannate dielectric material |
| CN107903059A (en) * | 2017-11-03 | 2018-04-13 | 天津大学 | A kind of intermediate sintering temperature microwave-medium ceramics and preparation method thereof |
| CN107935584A (en) * | 2017-12-12 | 2018-04-20 | 湖南先导电子陶瓷科技产业园发展有限公司 | A kind of microwave dielectric ceramic materials for LTCC and preparation method thereof |
| CN108610040A (en) * | 2018-04-27 | 2018-10-02 | 天津大学 | A method of reducing titanium barium stannate system dielectric loss under reducing atmosphere |
| CN108610041A (en) * | 2018-04-27 | 2018-10-02 | 天津大学 | A method of improving titanium barium stannate dielectric properties under reducing atmosphere |
| CN108727022A (en) * | 2018-07-04 | 2018-11-02 | 电子科技大学 | A kind of ultra-low loss magnesium-niobate lithium system microwave dielectric ceramic materials and preparation method thereof |
| CN108727022B (en) * | 2018-07-04 | 2020-11-27 | 电子科技大学 | Ultra-low-loss magnesium lithium niobate system microwave dielectric ceramic 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 |
| CN110655402A (en) * | 2019-10-14 | 2020-01-07 | 天津大学 | Medium-temperature sintered rutile-like microwave dielectric ceramic material |
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Application publication date: 20130501 |