CN107382306A - Applying acceptor cooperates with substitution to prepare ultrahigh Q-value microwave dielectric material - Google Patents

Applying acceptor cooperates with substitution to prepare ultrahigh Q-value microwave dielectric material Download PDF

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CN107382306A
CN107382306A CN201710508279.8A CN201710508279A CN107382306A CN 107382306 A CN107382306 A CN 107382306A CN 201710508279 A CN201710508279 A CN 201710508279A CN 107382306 A CN107382306 A CN 107382306A
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dielectric material
microwave dielectric
substitution
acceptor
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CN107382306B (en
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李玲霞
杜明昆
于仕辉
孙正
乔坚栗
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Tianjin University
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Abstract

Applying acceptor the invention discloses one kind cooperates with substitution to prepare ultrahigh Q-value microwave dielectric material, and synthetic expression formula is MgTi0.85(MxSb1‑x)0.15O3, wherein M is Na, Co or In, the x=1/4 as M=Na, the x=1/3 as M=Co, the x=1/2 as M=In.First by Na2CO3, CoO or In2O3With Sb2O5And TiO2Stoichiometrically formula Ti0.85(MxSb1‑x)0.15O3Dispensing is carried out, by ball milling, drying, is sieved after 1100~1300 DEG C of pre-burnings；After pre-burning again with MgO stoichiometrically formula MgTi0.85(MxSb1‑x)0.15O3Dispensing, then through ball milling, drying, sieve after 900~1100 DEG C of pre-burnings；Green compact are pressed into after being granulated again, ultrahigh Q-value microwave dielectric material is made then at 1300 DEG C~1400 DEG C sintering in green compact.Qf values of the present invention are up to 196,979~229,927GHz, while have higher ε concurrentlyrValue 16.69~16.88, is with a wide range of applications.

Description

Applying acceptor cooperates with substitution to prepare ultrahigh Q-value microwave dielectric material
Technical field
The invention belongs to a kind of ceramic composition characterized by composition, more particularly to a kind of ultrahigh Q-value microwave-medium material Material and preparation method thereof.
Background technology
Microstripline filter can effectively be filtered as the Primary Component in microwave circuit to the signal of specific frequency Remove, be widely used in the systems such as microwave communication, radar navigation, electronic countermeasure, satellite relay, missile guidance, test instrumentation.With Flourishing for information technology and wireless communication system, high-quality microstripline filter is towards low-loss, miniaturization, high frequency Change direction to develop.
High-quality microstripline filter be unable to do without the powerful support of high performance microwave medium substrate, is situated between using high q-factor microwave The substrate that material makes can reduce the insertion loss of wave filter, keep the integrality of data signal, ensure the excellent of frequency Selectivity, improves the working frequency of device, while be advantageous to simplify the heat radiation structure design of device.However, current high q-factor microwave Its Qf value of medium substrate material is generally in 100,000GHz or so, and dielectric constant is relatively low (＜ 10), can not still meet wave filter Low-loss, the demand of miniaturization.Therefore, ultrahigh Q-value microwave-medium baseplate material of the research and development with high dielectric constant has been compeled In the eyebrows and eyelashes.Wherein, MgTiO3Microwave dielectric material has excellent microwave dielectric property (ε in millimere-wave bandr~17.4, Qf~ 160,000GHz, τf~-55ppm/ DEG C), but in high-temperature sintering process, because relative partial pressure of oxygen reduces, part Ti4+It is reduced Into Ti3+, free electron and Lacking oxygen are supervened, while generate the second phase MgTi of dielectric properties difference2O5, severe exacerbation MgTiO3Qf values.Therefore, MgTiO is suppressed3Middle Ti4+Free electron and Lacking oxygen caused by high temperature reduction reaction, improve 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 suppress MgTiO3Microwave dielectric material is in high-temperature sintering process, part Ti4+It is reduced Into Ti3+, the free electron and Lacking oxygen supervened, while generate the second phase MgTi of dielectric properties difference2O5, so as to improve MgTiO3Qf values.
" electronics pinning " effect model is incorporated into microwave dielectric material design by the present invention, that is, utilizes donor ion Sb5+ With acceptor ion M=Na+、Co2+Or In3Collaboration substitution MgTiO3In Ti4+FormedCluster, will MgTiO3Microwave dielectric material is in high-temperature sintering process, due to Ti4+Reduction reaction caused by free electron and enliven oxygen sky Position localization, leakage electrical conduction current and dielectric loss is reduced, so as to by MgTiO under microwave frequency band3The Qf values of microwave dielectric material improve To 200,000GHz, there is provided a kind of ultrahigh Q-value microwave dielectric material.
The present invention is achieved by following technical solution.
One kind applies acceptor and cooperates with substitution to prepare ultrahigh Q-value microwave dielectric material, and target synthetic expression formula is MgTi0.85 (MxSb1-x)0.15O3, wherein M is Na, Co or In, the x=1/4 as M=Na, the x=1/3 as M=Co, the x=1/ as M=In 2；
The above-mentioned preparation method applied acceptor and cooperate with substitution to prepare ultrahigh Q-value microwave dielectric material, has following steps：
(1) by Na2CO3, CoO or In2O3With Sb2O5And TiO2Stoichiometrically formula Ti0.85(MxSb1-x)0.15O2Wherein M is Na, Co or In, the x=1/4 as M=Na, the x=1/3 as M=Co, as M=In, x=1/2 carries out dispensing, is put into polyester tank In, after adding deionized water and zirconium 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 the powder stoichiometrically formula MgTi after MgO and step (3) sieving0.85(MxSb1-x)0.15O3Wherein M is Na, Co or In, the x=1/4 as M=Na, the x=1/3 as M=Co, as M=In, x=1/2 carries out dispensing, is put into polyester tank In, after adding deionized water 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 900~1100 DEG C of pre-burnings, is incubated 2~8 hours, Then 40 mesh sieves are crossed；
(7) paraffin that the powder additional mass percent after step (6) is sieved is 8%~10% is carried out as adhesive It is granulated, crosses 80 mesh sieves, green compact are made with powder compressing machine pressure；
(8) by the green compact of step (7) in 1300 DEG C~1400 DEG C sintering, be incubated 2~8 hours, be made apply acceptor collaboration take The ultrahigh Q-value microwave dielectric material in generation.
The step (1), (4) carry out ball milling using planetary ball mill, and drum's speed of rotation is 400 revs/min.
The briquetting pressure of the step (7) is 4~8MPa.
The green compact a diameter of 10mm, thickness 5mm of the step (8).
The step (8) works as M=Na, and optimal sintering temperature during x=1/4 is 1325 DEG C, works as M=Co, during x=1/3 Optimal sintering temperature be 1350 DEG C, work as M=In, optimal sintering temperature during x=1/2 is 1375 DEG C.
The present invention is with MgO, TiO2And Sb2O5With Na2CO3, CoO or In2O3For raw material, prepare and apply the super of acceptor's collaboration substitution High q-factor microwave dielectric material MgTi0.85(MxSb1-x)0.15O3(x=1/ when x=1/3 when x=1/4 during M=Na, M=Co, M=In 2).Under microwave frequency band, the material product measures Qf values up to 196 under optimal sintering temperature, 979~229,927GHz, Quality factor with superelevation, ultralow dielectric loss, ceramic systems preparation technology are simple, it is not necessary to which high oxygen pressure atmosphere is burnt Knot, while have higher ε concurrentlyrIt is worth (16.69~16.88), the microwave-medium substrate being fabricated to is with a wide range of applications.
Embodiment
The present invention is more than 99% MgO, TiO with purity2And Sb2O5With Na2CO3, CoO or In2O3For initial feed, pass through Solid phase method prepares microwave dielectric material.Specific implementation step is as follows：
(1) by Na2CO3, CoO or In2O3With Sb2O5And TiO2Distinguish stoichiometrically formula Ti0.85(MxSb1-x)0.15O2(M is Na, Co or In, the x=1/4 as M=Na, the x=1/3 as M=Co, as M=In when x=1/2) carry out dispensing, raw material proportioning point It is not：①9.9672gTiO2、0.0863g Na2CO3、0.7965gSb2O5, 2. 9.9672gTiO2、0.3279gCoO、 1.4159gSb2O5, 3. 9.9672gTiO2、0.4512gIn2O3、0.5309gSb2O5.About 11g mixed powder is put into polyester In tank, 200ml deionized waters are added, after adding 150g zirconium ball, ball milling 12 hours on planetary ball mill, rotating speed 400 Rev/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 powder stoichiometrically formula MgTi after MgO and step (3) sieving0.85(MxSb1-x)0.15O3(M Na, Co Or In, the x=1/4 as M=Na, the x=1/3 as M=Co, as M=In when x=1/2) dispensing is carried out, raw material proportioning is respectively： ①5.3465gMgO、10.8561g Ti0.85(Na1/4Sb3/4)0.15O2, 2. 5.3465gMgO, 11.7112g Ti0.85(Co1/ 3Sb2/3)0.15O2, 3. 5.3465gMgO, 10.9493g Ti0.85(Na1/4Sb3/4)0.15O2, about 16g mixed powder is put into poly- In ester tank, after adding 200ml deionized waters and 150g zirconium ball, ball milling 12 hours；
(5) raw material after step (4) ball milling is respectively put into drying box, in 100~120 DEG C of drying, then crosses 40 mesh Sieve；
(6) powder after step (5) is sieved is respectively put into moderate oven, in 1000 DEG C of pre-burnings, is incubated 4 hours, then Cross 40 mesh sieves；
(7) paraffin that the powder additional mass percent after step (6) is sieved is 8% is granulated as adhesive, 80 mesh sieves are crossed, green compact are made with 4MPa pressure with powder compressing machine；
(8) by the green compact of step (8) respectively at 1300 DEG C -1400 DEG C sintering, be incubated 6 hours, be made apply acceptor collaboration take The ultrahigh Q-value microwave dielectric material in generation；
(9) microwave dielectric property of resulting product is tested by Network Analyzer.
Embodiment 1~15
The main technologic parameters and its microwave dielectric property of specific embodiment 1~15, refer to table 1.
Table 1

Claims (5)

  1. Substitution is cooperateed with to prepare ultrahigh Q-value microwave dielectric material 1. one kind applies acceptor, target synthetic expression formula is MgTi0.85 (MxSb1-x)0.15O3, wherein M is Na, Co or In, the x=1/4 as M=Na, the x=1/3 as M=Co, the x=1/ as M=In 2。
    The above-mentioned preparation method applied acceptor and cooperate with substitution to prepare ultrahigh Q-value microwave dielectric material, has following steps：
    (1) by Na2CO3, CoO or In2O3With Sb2O5And TiO2Stoichiometrically formula Ti0.85(MxSb1-x)0.15O2Wherein M is Na, Co Or In, the x=1/4 as M=Na, the x=1/3 as M=Co, as M=In, x=1/2 carries out dispensing, is put into polyester tank, adds After entering deionized water and zirconium 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 Cross 40 mesh sieves；
    (4) by the powder stoichiometrically formula MgTi after MgO and step (3) sieving0.85(MxSb1-x)0.15O3Wherein M be Na, Co or In, the x=1/4 as M=Na, the x=1/3 as M=Co, as M=In, x=1/2 carries out dispensing, is put into polyester tank, adds After deionized water 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 900~1100 DEG C of pre-burnings, is incubated 2~8 hours, then Cross 40 mesh sieves；
    (7) paraffin that the powder additional mass percent after step (6) is sieved is 8%~10% is made as adhesive Grain, 80 mesh sieves are crossed, green compact are made with powder compressing machine pressure；
    (8) green compact of step (7) are incubated 2~8 hours, are made and apply acceptor's collaboration substitution in 1300 DEG C~1400 DEG C sintering Ultrahigh Q-value microwave dielectric material.
  2. 2. it is according to claim 1 apply acceptor cooperate with substitution prepare ultrahigh Q-value microwave dielectric material, it is characterised in that institute It is 400 revs/min that step (1), (4), which are stated, using planetary ball mill progress ball milling, drum's speed of rotation.
  3. 3. it is according to claim 1 apply acceptor cooperate with substitution prepare ultrahigh Q-value microwave dielectric material, it is characterised in that institute The briquetting pressure for stating step (7) is 4~8MPa.
  4. 4. it is according to claim 1 apply acceptor cooperate with substitution prepare ultrahigh Q-value microwave dielectric material, it is characterised in that institute State the green compact a diameter of 10mm, thickness 5mm of step (8).
  5. 5. it is according to claim 1 apply acceptor cooperate with substitution prepare ultrahigh Q-value microwave dielectric material, it is characterised in that institute State the M=Na that works as of step (8), optimal sintering temperature during x=1/4 is 1325 DEG C, works as M=Co, optimal sintering during x=1/3 Temperature is 1350 DEG C, works as M=In, and optimal sintering temperature during x=1/2 is 1375 DEG C.
CN201710508279.8A 2017-06-28 2017-06-28 Preparation of ultra-high Q value microwave dielectric material by synergistic substitution of donor and acceptor Expired - Fee Related CN107382306B (en)

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CN110526711A (en) * 2019-09-10 2019-12-03 天津大学 Magnesium zirconium niobium tin tungsten series microwave dielectric ceramic and preparation method thereof
CN110698199A (en) * 2019-10-14 2020-01-17 天津大学 Low-loss microwave dielectric ceramic prepared by adopting step-by-step pre-firing method

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Cited By (3)

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Publication number Priority date Publication date Assignee Title
CN109970444A (en) * 2019-04-30 2019-07-05 天津大学 A kind of ultrahigh Q-value microwave dielectric material and preparation method thereof
CN110526711A (en) * 2019-09-10 2019-12-03 天津大学 Magnesium zirconium niobium tin tungsten series microwave dielectric ceramic and preparation method thereof
CN110698199A (en) * 2019-10-14 2020-01-17 天津大学 Low-loss microwave dielectric ceramic prepared by adopting step-by-step pre-firing method

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