CN107500750A - Magnesium niobium is co-doped with preparing high q-factor lithium-based microwave dielectric material - Google Patents
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Abstract
It is co-doped with preparing high q-factor lithium-based microwave dielectric material the invention discloses a kind of magnesium niobium, its chemical expression is Li2Ti1‑x(Mg1/ 3Nb2/3)xO3, wherein x=0.05~0.4.First by Li2CO3、TiO2, MgO and Nb2O5Stoichiometrically formula carries out dispensing, through ball milling, drying, in 700~900 DEG C of pre-burnings, additional 0.7w.t.% PVA powder is mixed, is granulated again, green compact are made with powder compressing machine in powder again, green compact are made magnesium niobium and are co-doped with preparing high q-factor lithium-based microwave dielectric material in 1200 DEG C~1300 DEG C sintering.The present invention is under microwave frequency band, product Qf values are up to 94,010GHz~115,424GHz, it is simple with low dielectric loss, preparation technology, it is not necessary to high oxygen pressure atmosphere sintering, dielectric constant (16.12~21.92) and temperature coefficient of resonance frequency (36.61~+7.96ppm/ DEG C) are adjustable simultaneously, and the microwave filter being made from it is with a wide range of applications.
Description
Technical field
The invention belongs to a kind of ceramic composition characterized by composition, more particularly to a kind of high q-factor lithium-based microwave medium
Material and preparation method thereof.
Background technology
Microwave filter can be effectively filtered out to the signal of specific frequency as the Primary Component in microwave circuit,
It is widely used in the systems such as microwave communication, radar navigation, electronic countermeasure, satellite relay, missile guidance, test instrumentation.With
Information technology and wireless communication system flourish, high-quality microwave wave filter must have good frequency selective characteristic and
Bandwidth, while develop towards miniaturization and cost degradation.
The microwave filter made using high q-factor microwave dielectric material, the insertion loss of device can be effectively reduced, improved
The corresponding degree of trembling and band efficiency of passband edge signal frequency, keep the integrality of data signal, ensure the excellent choosing of frequency
Selecting property, while be advantageous to simplify the heat radiation structure design of device.Wherein, there is the lithium base Li of rock salt structure2TiO3Microwave-medium material
Material has excellent microwave dielectric property (ε in millimere-wave bandr~22.14, Qf~63,525GHz, τf~+20.3ppm/ DEG C), it is former
Expect relatively cheap, preparation is simple, but it cleavage phenomenon easily occurs in (002) face, and surface has micro-crack, causes body
Product density is relatively low, at the same in high-temperature sintering process, because relative partial pressure of oxygen reduces, part Ti4+It is reduced into Ti3+, with production
Raw free electron, the above situation have had a strong impact on Li2TiO3Qf values.Therefore, Li is improved2TiO3Cleavage phenomenon and suppress Ti4+
Free electron caused by high temperature reduction reaction, improves its Qf value, turns into current urgent problem to be solved.
The content of the invention
The purpose of the present invention, it is to improve Li2TiO3The Qf values of microwave dielectric material, improve Li2TiO3Cleavage phenomenon and press down
Ti processed4+Free electron caused by high temperature reduction reaction.First, by MgO and Nb2O5It is incorporated into Li simultaneously2TiO3Microwave dielectric material
In design, on the one hand, utilize acceptor ion Mg2+Doping suppresses Ti4+Free electron caused by high temperature reduction reaction, reduce leakage and lead
Electric current and dielectric loss；On the other hand, Nb2O5Grain growth can be promoted, improve the microscopic appearance of material, reduce micro-crack
Produce, improve material volume density, while as Lacking oxygen caused by a kind of donor doping regulation and control acceptor doping.Finally, will
Li under microwave frequency band2TiO3The Qf values of microwave dielectric material are improved to 100,000GHz.
The present invention is achieved by following technical solution.
A kind of magnesium niobium is co-doped with preparing high q-factor lithium-based microwave dielectric material, and its chemical expression is Li2Ti1-x(Mg1/3Nb2/3)xO3, wherein x=0.05~0.4；
The preparation method of above-mentioned lithium-based microwave dielectric material, specific implementation step are as follows：
(1) by Li2CO3、TiO2, MgO and Nb2O5Stoichiometrically formula Li2Ti1-x(Mg1/3Nb2/3)xO3, wherein x=0.05
~0.4 carries out dispensing, and powder is put into polyester ball grinder, after adding absolute ethyl alcohol and zirconium ball, ball milling 4~24 hours；
(2) powder after step (1) ball milling is put into drying box, dried 4~6 hours in 100~120 DEG C, then mistake
40 mesh sieves；
(3) powder after step (2) is sieved is put into alumina crucible and is built in moderate oven, pre- in 700~900 DEG C
Burn, be incubated 2~8 hours, then cross 40 mesh sieves；
(4) the PVA powder of the additional 0.7w.t.% of powder after step (3) is sieved is mixed, and is put into polyester ball grinder
In, after adding absolute ethyl alcohol and zirconium ball, ball milling is granulated for 4~24 hours；
(5) by step (4) be granulated after powder be put into drying box, in 100~120 DEG C dry 4~6 hours, then
Cross 80 mesh sieves；
(6) green compact are made with 4~8MPa pressure with powder compressing machine in the powder after step (5) is sieved；
(7) green compact of step (6) are incubated 2~8 hours, magnesium niobium is made and is co-doped with preparing in 1200 DEG C~1300 DEG C sintering
High q-factor lithium-based microwave dielectric material.
The step (1), (4) carry out ball milling using planetary ball mill, and drum's speed of rotation is 400 revs/min.
The a diameter of 10mm of green compact of the step (6), thickness are 4~5mm.
The present invention is co-doped with (MgO and Nb using magnesium niobium2O5) prepare high q-factor lithium-based microwave medium material Li2Ti1-x(Mg1/ 3Nb2/3)xO3(x=0.05~0.4).Under microwave frequency band, product Qf values have up to 94,010GHz~115,424GHz
Low dielectric loss.The preparation technology of the microwave dielectric material system is simple, it is not necessary to high oxygen pressure atmosphere sintering, while dielectric is normal
Number (16.12~21.92) and temperature coefficient of resonance frequency (- 36.61~+7.96ppm/ DEG C) are adjustable, the microwave filter being made from it
Ripple utensil has wide practical use.
Embodiment
The present invention is more than 99% Li with purity2CO3、TiO2, MgO and Nb2O5For initial feed, prepared by solid phase method
Microwave dielectric material.Specific implementation step is as follows：
(1) by Li2CO3、TiO2, MgO and Nb2O5Stoichiometrically formula Li2Ti1-x(Mg1/3Nb2/3)xO3, wherein x=0.05
~0.4 carries out dispensing, and powder is put into polyester ball grinder, after adding absolute ethyl alcohol and zirconium ball, ball milling 4~24 hours；
Ball milling is carried out using planetary ball mill, drum's speed of rotation is 400 revs/min；
(2) powder after step (1) ball milling is put into drying box, dried 4~6 hours in 100~120 DEG C, then mistake
40 mesh sieves；
(3) powder after step (2) is sieved is put into alumina crucible and is built in moderate oven, pre- in 700~900 DEG C
Burn, be incubated 2~8 hours, then cross 40 mesh sieves；
(4) the PVA powder of the additional 0.7w.t.% of powder after step (3) is sieved is mixed, and is put into polyester ball grinder
In, after adding absolute ethyl alcohol and zirconium ball, ball milling is granulated for 4~24 hours；
Ball milling is carried out using planetary ball mill, drum's speed of rotation is 400 revs/min；
(5) by step (4) be granulated after powder be put into drying box, in 100~120 DEG C dry 4~6 hours, then
Cross 80 mesh sieves；
(6) green compact are made with 4~8MPa pressure with powder compressing machine in the powder after step (5) is sieved；
The a diameter of 10mm of green compact, thickness are 4~5mm；
(7) green compact of step (6) are incubated 2~8 hours, magnesium niobium is made and is co-doped with preparing in 1200 DEG C~1300 DEG C sintering
High q-factor lithium-based microwave dielectric material.
(8) as Network Analyzer test obtained by sample microwave dielectric property.
Li of the present invention2Ti1-x(Mg1/3Nb2/3)xO3The raw material proportioning of specific embodiment refers to table 1.
(the unit of table 1：g)
| Embodiment | x | Li2CO3 | TiO2 | MgO | Nb2O5 |
| 1 | 0.05 | 7.5399 | 7.6671 | 0.0685 | 0.3897 |
| 2 | 0.1 | 7.5399 | 7.2635 | 0.1371 | 0.7794 |
| 3 | 0.15 | 7.5399 | 6.8599 | 0.2056 | 1.1692 |
| 4 | 0.2 | 7.5399 | 6.4564 | 0.2742 | 1.5589 |
| 5 | 0.3 | 7.5399 | 5.6494 | 0.4113 | 2.3383 |
| 6 | 0.4 | 7.5399 | 4.8424 | 0.5484 | 3.1178 |
Microwave dielectric property of the specific embodiment of the invention under different sintering temperatures refers to table 2.
Table 2
Different content magnesium niobium is co-doped with the Li prepared2TiO3Microwave dielectric material, its Qf value is than pure phase Li2TiO3Have
Significantly lifted, in x=0.2,1300 DEG C of sintering, it is 115,424GHz that product, which has highest Qf values, for practical application
In demand, the content that can be co-doped with by adjusting magnesium niobium, to meet dielectric constant (16.12~21.92) and resonant frequency temperature
Spend the requirement of coefficient (- 36.61~+7.96ppm/ DEG C).
The invention is not limited in above-described embodiment, the change of many details is possible, but therefore this does not run counter to this
The scope and spirit of invention.
Claims (3)
1. a kind of magnesium niobium is co-doped with preparing high q-factor lithium-based microwave dielectric material, its chemical expression is Li2Ti1-x(Mg1/3Nb2/3)xO3, wherein x=0.05~0.4.
The preparation method of above-mentioned lithium-based microwave dielectric material, specific implementation step are as follows：
(1) by Li2CO3、TiO2, MgO and Nb2O5Stoichiometrically formula Li2Ti1-x(Mg1/3Nb2/3)xO3, wherein x=0.05~0.4
Dispensing is carried out, powder is put into polyester ball grinder, after adding absolute ethyl alcohol and zirconium ball, ball milling 4~24 hours；
(2) powder after step (1) ball milling is put into drying box, is dried in 100~120 DEG C 4~6 hours, then cross 40 mesh
Sieve；
(3) powder after step (2) is sieved is put into alumina crucible and is built in moderate oven, in 700~900 DEG C of pre-burnings, protects
Temperature 2~8 hours, then cross 40 mesh sieves；
(4) the PVA powder of the additional 0.7w.t.% of powder after step (3) is sieved is mixed, and is put into polyester ball grinder,
After adding absolute ethyl alcohol and zirconium ball, ball milling is granulated for 4~24 hours；
(5) powder after step (4) is granulated is put into drying box, is dried in 100~120 DEG C 4~6 hours, is then crossed 80
Mesh sieve；
(6) green compact are made with 4~8MPa pressure with powder compressing machine in the powder after step (5) is sieved；
(7) green compact of step (6) are incubated 2~8 hours, magnesium niobium is made and is co-doped with preparing high q-factor in 1200 DEG C~1300 DEG C sintering
Lithium-based microwave dielectric material.
2. it is co-doped with preparing high q-factor lithium-based microwave dielectric material according to the magnesium niobium described in claim 1, it is characterised in that described
Step (1), (4) carry out ball milling using planetary ball mill, and drum's speed of rotation is 400 revs/min.
3. it is co-doped with preparing high q-factor lithium-based microwave dielectric material according to the magnesium niobium described in claim 1, it is characterised in that described
The a diameter of 10mm of green compact of step (6), thickness are 4~5mm.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108975905A (en) * | 2018-08-16 | 2018-12-11 | 天津大学 | A kind of xenogenesis oxide is co-doped with the preparation method of lithium titanate base microwave dielectric material |
| CN109111225A (en) * | 2018-08-16 | 2019-01-01 | 天津大学 | Regulate and control the lithium titanate base microwave dielectric material of microwave dielectric property by magnesium niobium component |
| CN109912306A (en) * | 2019-03-06 | 2019-06-21 | 天津大学 | A kind of adjustable high q-factor microwave-medium ceramics of temperature coefficient of resonance frequency |
| CN113979743A (en) * | 2021-10-08 | 2022-01-28 | 天津大学 | high-Q light microwave dielectric ceramic for 5G base station ceramic filter and preparation method thereof |
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| CN101260001A (en) * | 2008-02-29 | 2008-09-10 | 上海大学 | High-Q microwave dielectric ceramic material and preparing method thereof |
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2017
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101260001A (en) * | 2008-02-29 | 2008-09-10 | 上海大学 | High-Q microwave dielectric ceramic material and preparing method thereof |
| CN106007707A (en) * | 2016-07-05 | 2016-10-12 | 天津大学 | Mg-Nb doped bismuth titanate microwave dielectric ceramic and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108975905A (en) * | 2018-08-16 | 2018-12-11 | 天津大学 | A kind of xenogenesis oxide is co-doped with the preparation method of lithium titanate base microwave dielectric material |
| CN109111225A (en) * | 2018-08-16 | 2019-01-01 | 天津大学 | Regulate and control the lithium titanate base microwave dielectric material of microwave dielectric property by magnesium niobium component |
| CN109912306A (en) * | 2019-03-06 | 2019-06-21 | 天津大学 | A kind of adjustable high q-factor microwave-medium ceramics of temperature coefficient of resonance frequency |
| CN113979743A (en) * | 2021-10-08 | 2022-01-28 | 天津大学 | high-Q light microwave dielectric ceramic for 5G base station ceramic filter and preparation method thereof |
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