CN107573057A - A kind of combined temp stable type high q-factor microwave dielectric material - Google Patents
A kind of combined temp stable type high q-factor microwave dielectric material Download PDFInfo
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Abstract
The invention discloses a kind of combined temp stable type high q-factor microwave dielectric material, target synthetic expression formula is (1 x) MgTiO3‑x Li2Ti0.85(Al1/2Nb1/2)0.15O3, wherein x=0.1~0.7.First by MgO and TiO2Stoichiometrically formula prepares MgTiO3, then by Li2CO3、TiO2、Al2O3And Nb2O5Stoichiometrically formula prepares Li2Ti0.85(Al1/2Nb1/2)0.15O3；Again by MgTiO3And Li2Ti0.85(Al1/2Nb1/2)0.15O3Stoichiometrically formula carries out dispensing, then additional 0.5~1w.t.% PVA powder is mixed, and through ball milling, drying, sieving, pressure system is shaped to base substrate, and combined temp stable type high q-factor microwave dielectric material is made in 1175 DEG C of 1275 DEG C of sintering in base substrate.The present invention | τf|≤10ppm/ DEG C, there is nearly zero temperature coefficient of resonance frequency, there is higher Q × f values 30,913~45,210GHz, preparation technology is simple, is with a wide range of applications.
Description
Technical field
The present invention is micro- on electronic information material and component, more particularly to a kind of New temperature stable type high q-factor
Ripple dielectric material and preparation method thereof
Background technology
The continuous development of modern communication technology, to the minimizing of component, it is integrated and it is modular require increasingly urgent,
Higher requirement is proposed to microwave dielectric material.The microwave dielectric material of microwave dielectric material especially perovskite structure into
For one of most active functional material in recent years.Wherein, MgTiO3Ceramics are as a kind of microwave of traditional perovskite-like structure
Dielectric material, there is the excellent microwave dielectric properties such as low-k, high quality factor in microwave frequency band, can effectively subtract
The signal delay of gadget simultaneously keeps signal integrity.However, there is the poor (τ of temperature stability in itf~-50ppm/ DEG C), sintering
The shortcomings that temperature height (1400 DEG C of ＞).
Microwave device needs to work under different environment temperatures, as material τfWhen value is very big, the center resonance frequency of device
Rate will have very big drift with the change of temperature, causes device normally to work, typically requires material | τf|≤
10ppm/ DEG C, i.e. the temperature coefficient of resonance frequency of microwave dielectric material needs nearly zero, so just can ensure that prepared device tool
There are high reliability and high stability.Therefore, MgTiO3The research of base microwave dielectric material temperature stability turns into a big focus.
Regulation MgTiO in the past3The mode of temperature stability can deteriorate its quality factor, therefore study a kind of high Q of New temperature stable type
The MgTiO of value3Base microwave dielectric material is increasingly urgent.
The content of the invention
The purpose of the present invention is to overcome some additives (such as CaTiO3、SrTiO3Deng) regulation MgTiO3 system temperature stabilizations
After property, the shortcomings that Q values are greatly reduced and sintering temperature is higher and deficiency, creatively by Li2TiO3Base microwave dielectric material introduces
To MgTiO3In the design of system temperature stability, that is, utilize Li2Ti0.85(Al1/2Nb1/2)0.15O3Adjust MgTiO3Microwave-medium
The temperature stability of material, meanwhile, Li2TiO3MgTiO can also be reduced3The sintering temperature of (1400 DEG C of ＞), passes through MgTiO3-
Li2Ti0.85(Al1/2Nb1/2)0.15O3The microwave dielectric material of synthesizing new temperature-stable high q-factor coexists in complex phase.
The present invention is achieved by following technical solution.
A kind of combined temp stable type high q-factor microwave dielectric material, target synthetic expression formula are (1-x) MgTiO3-
xLi2Ti0.85(Al1/2Nb1/2)0.15O3, wherein x=0.1~0.7.
The preparation method of the combined temp stable type high q-factor microwave dielectric material, specific implementation step are as follows：
(1) by MgO and TiO2Stoichiometrically formula MgTiO3Dispensing is carried out, is put into polyester tank, adds deionized water and zirconium
After ball, ball milling 4~24 hours；
(2) raw material after step (1) ball milling is put into drying box, in 100~120 DEG C of drying, then crosses 40 mesh sieves；
(3) powder after step (2) is sieved is put into moderate oven, in 1100~1300 DEG C of pre-burnings, is incubated 2~8 hours,
Then 40 mesh sieves are crossed；
(4) by Li2CO3、TiO2、Al2O3And Nb2O5Stoichiometrically formula Li2Ti0.85(Al1/2Nb1/2)0.15O3Carry out dispensing,
It is put into polyester tank, after adding absolute ethyl alcohol and zirconium ball, ball milling 4~24 hours；
(5) raw material after step (4) ball milling is put into drying box, in 100~120 DEG C of drying, then crosses 40 mesh sieves；
(6) powder after step (5) is sieved is put into moderate oven, in 800~1000 DEG C of pre-burnings, is incubated 2~8 hours,
Then 40 mesh sieves are crossed；
(7) by powder stoichiometrically formula (1-x) MgTiO after step (3) and (6) sieving3-xLi2Ti0.85(Al1/ 2Nb1/2)0.15O3Wherein x=0.1~0.7 carries out dispensing, then additional 0.5~1w.t.% PVA powder is mixed, mixed powder
Material is put into polyester tank, after absolute ethyl alcohol and zirconium ball are removed in addition, ball milling 4~24 hours；
(8) raw material after step (7) ball milling is put into drying box, in 100~120 DEG C of drying, then crosses 80 mesh sieves；
(9) green compact are made with 4~8MPa pressure with powder compressing machine in the powder of step (8)；
(10) green compact of step (9) are incubated 2~8 hours, it is stable that combined temp is made in 1175 DEG C of -1275 DEG C of sintering
Type high q-factor microwave dielectric material.
The step (1), (4) or (7) carries 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 (9), thickness are 4~5mm.
The sintering temperature of the step (10) is 1250 DEG C.
The present invention is with MgO, TiO2、Li2CO3、Al2O3、Nb2O5NEW TYPE OF COMPOSITE MgTiO is prepared for raw material3-Li2Ti0.85
(Al1/2Nb1/2)0.15O3Temperature-stable high q-factor microwave dielectric material.Under microwave frequency band, the material sample is in optimal sintering temperature
Under, measure | τf|≤10ppm/ DEG C, have nearly zero temperature coefficient of resonance frequency, while have concurrently higher Q × f values 30,913~
45,210GHz, ceramic systems preparation technology is simple, is with a wide range of applications.
Embodiment
The present invention is more than 99% MgO, TiO with purity2、Li2CO3、Al2O3And Nb2O5For initial feed, pass through solid phase method
Prepare microwave dielectric material.Specific embodiment is as follows：
By MgO, Li2CO3、TiO2、Al2O3And Nb2O5Dispensing is carried out by following stoichiometric equation：
①MgTiO3、②Li2Ti0.85(Al1/2Nb1/2)0.15O3、③0.5MgTiO3-0.5Li2Ti0.85(Al1/2Nb1/2)0.15O3Specific proportioning refers to table 1, table 2, table 3.
The MgTiO of table 13List of ingredients (unit：g)
| MgO | TiO2 |
| 3.3530 | 6.6470 |
The Li of table 22Ti0.85(Al1/2Nb1/2)0.15O3List of ingredients (unit：g)
| Li2CO3 | TiO2 | Al2O3 | Nb2O5 |
| 4.9009g | 4.4590g | 0.2510g | 0.6480g |
The 0.5MgTiO of table 33-0.5Li2Ti0.85(Al1/2Nb1/2)0.15O3List of ingredients (unit：g)
| MgTiO3 | Li2Ti0.85(Al1/2Nb1/2)0.15O3 |
| 3.3530 | 6.6470 |
(1) by the MgTiO in table 13Mixed powder is put into polyester tank, adds 200ml deionized waters, adds 150g zirconium
After ball, ball milling 12 hours on planetary ball mill, rotating speed is 400 revs/min；
(2) raw material after step (1) ball milling is respectively put into drying box, in 100~120 DEG C of drying, then crosses 40 mesh
Sieve；
(3) powder after step (2) is sieved is put into moderate oven, in 1100 DEG C of pre-burnings, is incubated 4 hours, is then crossed 40
Mesh sieve；
(4) by the Li in table 22Ti0.85(Al1/2Nb1/2)0.15O3Mixed powder is put into polyester tank, is added 200ml and is gone nothing
Water-ethanol, after adding 150g zirconium ball, ball milling 12 hours on planetary ball mill, rotating speed is 400 revs/min；
(5) raw material after step (4) ball milling is put into drying box, in 100~120 DEG C of drying, then crosses 40 mesh sieves；
(6) powder after step (5) is sieved is put into moderate oven, in 1000 DEG C of pre-burnings, is incubated 4 hours, is then crossed 40
Mesh sieve；
(7) powder after step (3) and (6) sieving is subjected to dispensing, then additional 0.7w.t.% PVA powder by table 3,
Mixed powder is put into polyester tank, after addition 200ml removes absolute ethyl alcohol and 150g zirconium ball, ball milling 24 hours；
(8) raw material after step (7) ball milling is put into drying box, in 100~120 DEG C of drying, then crosses 80 mesh sieves；
(9) green compact are made with 4MPa pressure with powder compressing machine in the powder of step (8)；
(10) green compact of step (9) are incubated 6 hours in 1175 DEG C of -1275 DEG C of sintering.
(11) as Network Analyzer test obtained by sample microwave dielectric property.
The main technologic parameters and its microwave dielectric property of the specific embodiment of the invention refer to table 4.
Table 4
Claims (4)
1. a kind of combined temp stable type high q-factor microwave dielectric material, target synthetic expression formula is (1-x) MgTiO3-
xLi2Ti0.85(Al1/2Nb1/2)0.15O3, wherein x=0.1~0.7.
The preparation method of the combined temp stable type high q-factor microwave dielectric material, specific implementation step are as follows：
(1) by MgO and TiO2Stoichiometrically formula MgTiO3Dispensing is carried out, is put into polyester tank, adds deionized water and zirconium ball
Afterwards, ball milling 4~24 hours；
(2) raw material after step (1) ball milling is put into drying box, in 100~120 DEG C of drying, then crosses 40 mesh sieves；
(3) powder after step (2) is sieved is put into moderate oven, in 1100~1300 DEG C of pre-burnings, is incubated 2~8 hours, then
Cross 40 mesh sieves；
(4) by Li2CO3、TiO2、Al2O3And Nb2O5Stoichiometrically formula Li2Ti0.85(Al1/2Nb1/2)0.15O3Dispensing is carried out, is put into
In polyester tank, after adding absolute ethyl alcohol and zirconium ball, ball milling 4~24 hours；
(5) raw material after step (4) ball milling is put into drying box, in 100~120 DEG C of drying, then crosses 40 mesh sieves；
(6) powder after step (5) is sieved is put into moderate oven, in 800~1000 DEG C of pre-burnings, is incubated 2~8 hours, then
Cross 40 mesh sieves；
(7) by powder stoichiometrically formula (1-x) MgTiO after step (3) and (6) sieving3-xLi2Ti0.85(Al1/2Nb1/2)0.15O wherein x=0.1~0.7 carries out dispensing, then additional 0.5~1w.t.% PVA powder is mixed, and mixed powder is put into
In polyester tank, after absolute ethyl alcohol and zirconium ball are removed in addition, ball milling 4~24 hours；
(8) raw material after step (7) ball milling is put into drying box, in 100~120 DEG C of drying, then crosses 80 mesh sieves；
(9) green compact are made with 4~8MPa pressure with powder compressing machine in the powder of step (8)；
(10) green compact of step (9) are incubated 2~8 hours, the high Q of combined temp stable type is made in 1175 DEG C of -1275 DEG C of sintering
It is worth microwave dielectric material.
2. a kind of combined temp stable type high q-factor microwave dielectric material according to claim 1, it is characterised in that described
Step (1), (4) or (7) carries out ball milling using planetary ball mill, and drum's speed of rotation is 400 revs/min.
3. a kind of combined temp stable type high q-factor microwave dielectric material according to claim 1, it is characterised in that described
The a diameter of 10mm of green compact of step (9), thickness are 4~5mm.
4. a kind of combined temp stable type high q-factor microwave dielectric material according to claim 1, it is characterised in that described
The sintering temperature of step (10) is 1250 DEG C.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115490512A (en) * | 2022-09-19 | 2022-12-20 | 大富科技(安徽)股份有限公司 | 5G microwave dielectric ceramic material, preparation method thereof and microwave dielectric ceramic device |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104844193A (en) * | 2015-04-08 | 2015-08-19 | 天津大学 | Lithium-magnesium-titanium-based microwave dielectric ceramic with high Q value and low temperature sintering realization method thereof |
| CN104961467A (en) * | 2015-06-12 | 2015-10-07 | 华南理工大学 | High-toughness ceramic matrix composite and preparing method and application thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104844193A (en) * | 2015-04-08 | 2015-08-19 | 天津大学 | Lithium-magnesium-titanium-based microwave dielectric ceramic with high Q value and low temperature sintering realization method thereof |
| CN104961467A (en) * | 2015-06-12 | 2015-10-07 | 华南理工大学 | High-toughness ceramic matrix composite and preparing method and application thereof |
Non-Patent Citations (3)
| Title |
|---|
| HUANFU ZHOU等: "Preparation, phase structure and microwave dielectric properties of a new low cost MgLi2/3Ti4/3O4 compound", 《MATERIALS CHEMISTRY AND PHYSICS》 * |
| YI-DING ZHANG等: "Pseudo Phase Diagram and Microwave Dielectric Properties of Li2O–MgO–TiO2 Ternary System", 《JOURNAL OF THE AMERICAN CERAMIC SOCIETY》 * |
| ZHANG TIANWEN等: "Structure, Microwave Dielectric Properties, and Low-Temperature Sintering of Acceptor/Donor Codoped Li2Ti1-x(Al0.5Nb0.5)xO3 Ceramics", 《JOURNAL OF THE AMERICAN CERAMIC SOCIETY》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115490512A (en) * | 2022-09-19 | 2022-12-20 | 大富科技(安徽)股份有限公司 | 5G microwave dielectric ceramic material, preparation method thereof and microwave dielectric ceramic device |
| CN115490512B (en) * | 2022-09-19 | 2023-10-20 | 大富科技(安徽)股份有限公司 | 5G microwave dielectric ceramic material, preparation method thereof and microwave dielectric ceramic device |
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