CN105859289A - Low-temperature sintering low-loss magnesium-lithium-niobate-series microwave dielectric ceramic - Google Patents

Low-temperature sintering low-loss magnesium-lithium-niobate-series microwave dielectric ceramic Download PDF

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CN105859289A
CN105859289A CN201610414620.9A CN201610414620A CN105859289A CN 105859289 A CN105859289 A CN 105859289A CN 201610414620 A CN201610414620 A CN 201610414620A CN 105859289 A CN105859289 A CN 105859289A
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microwave dielectric
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张平
刘路
赵永贵
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Tianjin University
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Abstract

The invention provides a low-temperature sintering low-loss magnesium-lithium-niobate-series microwave dielectric ceramic. On the basis of a Li3Mg2NbO6 microwave dielectric ceramic, 0.5%-3% of ZBS (60 wt% of ZnO, 30 wt% of B2O3 and 10 wt% of SiO2) sintering aid is additionally added, and the sintering temperature is successfully reduced to 925 DEG C from 1,250 DEG C. The performance of the prepared Li3Mg2NbO6 microwave dielectric ceramic is tested, and good microwave dielectric characteristics that the relative dielectric constant is 14.30, the quality factor is 73, 987 GHz, and the temperature coefficient of resonance frequency is -16.05 ppm/DEG C are achieved. The preparation process is simple, the course is free of contamination, the temperature coefficient of resonance frequency is increased, and the low-temperature sintering low-loss magnesium-lithium-niobate-series microwave dielectric ceramic is a promising LTCC microwave dielectric material.

Description

A kind of low-temperature sintering low-loss lithium magnesium niobium series microwave dielectric ceramic
Technical field
The invention belongs to a kind of ceramic composition being characterized with composition, particularly to a kind of new type low temperature sintering low-loss Li3Mg2NbO6Series microwave dielectric ceramic and preparation method thereof.
Background technology
Along with microwave communication in the present age and the developing rapidly of wireless communication industry, it is desirable to all kinds of microwave devices to miniaturization, lightweight, Integrated and cost degradation direction is developed.With LTCC (low-temperature co-fired ceramic, LTCC) Multi-layer structure design based on technology can effectively reduce device volume, is to realize microwave device miniaturization, integrated and mould The important channel of block.
In order to realize the sandwich construction of LTCC technology, it is desirable to microwave dielectric material can be with high conductivity and cheap silver electrode (961 DEG C) realize burning altogether.It is therefore desirable to the sintering temperature for use microwave dielectric material on microwave device will be 950 Below DEG C.Generally adding low melting point oxide or glass sintering auxiliary agent is most common to reduce the sintering temperature of microwave dielectric material A kind of method reducing sintering temperature.
Li3Mg2NbO6Being a kind of novel microwave dielectric material with superior microwave dielectric property, its dielectric constant is 16.8, Q × f value is 79,643GHz, and temperature coefficient of resonance frequency is-27.2ppm/ DEG C, but sintering temperature is 1250 DEG C. Its higher sintering temperature limits its application on LTCC.The present invention uses conventional solid-state method, by pre-burning pottery Powder adds sintering aid, prepares low sintering Li3Mg2NbO6Microwave-medium ceramics so that it is meet at LTCC The application of technology.
Summary of the invention
The purpose of the present invention, is to overcome existing Li3Mg2NbO6Series microwave dielectric ceramic sintering temperature is too high, limit it The defect of the upper application of LTCC, it is provided that a kind of with Li2CO3、MgO、Nb2O5For primary raw material, additional a small amount of ZBS (60 Wt%ZnO 30wt%B2O310wt%SiO2) glass as sintering aid, make Li3Mg2NbO6Series microwave dielectric is made pottery Porcelain sintering temperature is reduced to less than 950 DEG C, keeps the microwave dielectric property of its excellence simultaneously.
The present invention is achieved by following technical solution.
1. a low-temperature sintering low-loss lithium magnesium niobium series microwave dielectric ceramic, its chemical formula is Li3Mg2NbO6, basis at this The ZBS sintering aid of upper additional 0.5%~3%;
Described ZBS sintering aid is 60wt%ZnO 30wt%B2O310wt%SiO2
The preparation method of this low-temperature sintering low-loss lithium magnesium niobium series microwave dielectric ceramic, has following steps:
(1) with Li2CO3、MgO、Nb2O5For raw material, by Li3Mg2NbO6Stoichiometric proportion carry out weigh dispensing, press Raw material: deionized water: the ratio of abrading-ball=2:16:15 adds in polyester tank, ball milling 6 hours on ball mill;
(2) raw material after step (1) ball milling is put in baking oven, dries at 120 DEG C, grind and then cross 40 mesh sieves, it is thus achieved that Evengranular powder;
(3) powder that step (2) mixes is placed in crucible in 1050 DEG C of calcinings, is incubated 4 hours;
(4) ceramic powder after step (3) is calcined is put in polyester tank, and additional mass percent is the ZBS of 0.5%~3%, It is subsequently adding deionized water and zirconia ball, ball milling 6 hours on ball mill;After drying in ceramic powder additional quality hundred Proportion by subtraction be 8% paraffin carry out granulation as adhesive, cross 80 mesh sieves, then be shaped to base substrate with powder compressing machine;
(5) by step (4) in base substrate at 850~950 DEG C of sintering, be incubated 4 hours, heating rate is 5 DEG C/min, prepare Low-temperature sintering low-loss Li3Mg2NbO6Series microwave dielectric ceramic.
The Li of described step (1)2CO3、MgO、Nb2O5The quality purity of raw material is more than 99.9%.
The mass percent of the additional ZBS of described step (4) is 1.0%.
The operating pressure of the tablet press machine of described step (4) is 2MPa, and base substrate specification is the cylinder of Φ 10mm × 5mm.
The sintering temperature of described step (5) is 925 DEG C.
The present invention is with Li3Mg2NbO6Based on microwave-medium ceramics, add ZBS (60wt%ZBS 30wt%B2O3– 10wt%SiO2) sintering aid, successfully its sintering temperature is down to 925 DEG C by 1250 DEG C, prepare dielectric constant be 14.30, Quality factor 73,987GHz, temperature coefficient of resonance frequency are the microwave-medium ceramics of-16.05ppm/ DEG C.The preparation of the present invention Technique is simple, and process is pollution-free, improves its temperature coefficient of resonance frequency, is a kind of up-and-coming LTCC microwave-medium Material.
Detailed description of the invention
The present invention uses the chemical raw material Li that purity is more than 99.9%2CO3、MgO、Nb2O5Preparation Li3Mg2NbO6Microwave Media ceramic.
The present invention is by Li2CO3、MgO、Nb2O5Chemical formula Li pressed by raw material3Mg2NbO6Stoichiometric proportion carry out dispensing, With raw material: deionized water: the ratio of abrading-ball=2:16:15 adds in polyester tank, ball milling 6 hours;Raw material after ball milling is placed in baking In 120 DEG C of drying in case, cross 40 mesh sieves, calcine 4 hours then at 1050 DEG C;Again the ceramic powder after calcining is put into ball In grinding jar, weigh ZBS (the 60wt%ZnO 30wt%B that mass percent is 0.5%-3%2O310wt%SiO2) Sintering aid adds in the powder after calcining, is subsequently adding zirconia ball and 6 hours post-dryings of deionized water ball milling;Drying again In ceramic powder after Gan added weight percentage be 8% paraffin wax binder carry out granulation, after crossing 80 mesh sieves, use powder pressure Powder is pressed into a diameter of 10mm under the pressure of 2MPa by sheet machine, and thickness is the green compact of 5mm;By green compact at 850~950 DEG C Sintering, is incubated 4 hours, prepares low-temperature sintering low-loss microwave-medium ceramics;Finally by Network Analyzer and dependence test The microwave dielectric property of fixture test article.
The specific embodiment of the invention is as follows.
Embodiment 1:
1. according to microwave-medium ceramics component Li3Mg2NbO6, claim Li2CO3-6.8344g、MgO-4.9705g、Nb2O5- -8.1951g dispensing, altogether 20g;Mixed powder adds in polyester tank, after adding 160ml deionized water and 150g zirconium ball, Ball milling 6 hours on planetary ball mill, drum's speed of rotation is 1000 revs/min;
2. the raw material after ball milling is placed in drying box, dries in 120 DEG C and cross 40 mesh sieves, it is thus achieved that evengranular powder;
3. powder is calcined 4 hours in 1050 DEG C;
4. the powder after calcining is put in polyester tank, then after weighing ZBS-0.0200g that mass fraction is 0.1% and calcining Powder mixing, secondary ball milling 6 hours, discharging post-drying, cross 40 mesh sieves;It is subsequently adding the stone that percentage by weight is 8% Wax carries out granulation as adhesive, and crosses 80 mesh sieves;It is pressed into a diameter of 10mm with the pressure of 2MPa again with powder compressing machine, Thickness is the base substrate of 5mm;
5. by base substrate in 850 DEG C of sintering, it is incubated 4 hours, prepares low-temperature sintering low-loss microwave-medium Li3Mg2NbO6Pottery Porcelain;
Finally, gained sample microwave property is tested by Network Analyzer and dependence test fixture.
Embodiment 2:
1. according to microwave-medium ceramics component Li3Mg2NbO6, claim Li2CO3-6.8344g、MgO-4.9705g、Nb2O5- -8.1951g dispensing, altogether 20g;Mixed powder adds in polyester tank, after adding 160ml deionized water and 150g zirconium ball, Ball milling 6 hours on planetary ball mill, drum's speed of rotation is 1000 revs/min;
2. the raw material after ball milling is placed in drying box, dries in 120 DEG C and cross 40 mesh sieves, it is thus achieved that evengranular powder;
3. powder is calcined 4 hours in 1050 DEG C;
4. the powder after calcining is put in polyester tank, then after weighing ZBS-0.1000g that mass fraction is 0.5% and calcining Powder mixing, secondary ball milling 6 hours, discharging post-drying, cross 40 mesh sieves;It is subsequently adding the stone that percentage by weight is 8% Wax carries out granulation as adhesive, and crosses 80 mesh sieves;It is pressed into a diameter of 10mm with the pressure of 2MPa again with powder compressing machine, Thickness is the base substrate of 5mm;
5. by base substrate in 850 DEG C of sintering, it is incubated 4 hours, prepares low-temperature sintering low-loss microwave-medium Li3Mg2NbO6Pottery Porcelain;
Finally, gained sample microwave property is tested by Network Analyzer and dependence test fixture.
Embodiment 3:
1. according to microwave-medium ceramics component Li3Mg2NbO6, claim Li2CO3-6.8344g、MgO-4.9705g、Nb2O5- -8.1951g dispensing, altogether 20g;Mixed powder adds in polyester tank, after adding 160ml deionized water and 150g zirconium ball, Ball milling 6 hours on planetary ball mill, drum's speed of rotation is 1000 revs/min;
2. the raw material after ball milling is placed in drying box, dries in 120 DEG C and cross 40 mesh sieves, it is thus achieved that evengranular powder;
3. powder is calcined 4 hours in 1050 DEG C;
4. the powder after calcining is put in polyester tank, then after weighing ZBS-0.2000g that mass fraction is 1% and calcining Powder mixes, secondary ball milling 6 hours, discharging post-drying, crosses 40 mesh sieves;It is subsequently adding the paraffin that percentage by weight is 8% Carry out granulation as adhesive, and cross 80 mesh sieves;It is pressed into a diameter of 10mm with the pressure of 2MPa again with powder compressing machine, Thickness is the base substrate of 5mm;
5. by base substrate in 850 DEG C of sintering, it is incubated 4 hours, prepares low-temperature sintering low-loss microwave-medium Li3Mg2NbO6Pottery Porcelain;
Finally, gained sample microwave property is tested by Network Analyzer and dependence test fixture.
Embodiment 4:
1. according to microwave-medium ceramics component Li3Mg2NbO6, claim Li2CO3-6.8344g、MgO-4.9705g、Nb2O5- -8.1951g dispensing, altogether 20g;Mixed powder adds in polyester tank, after adding 160ml deionized water and 150g zirconium ball, Ball milling 6 hours on planetary ball mill, drum's speed of rotation is 1000 revs/min;
2. the raw material after ball milling is placed in drying box, dries in 120 DEG C and cross 40 mesh sieves, it is thus achieved that evengranular powder;
3. powder is calcined 4 hours in 1050 DEG C;
4. the powder after calcining is put in polyester tank, then after weighing ZBS-0.4000g that mass fraction is 2% and calcining Powder mixes, secondary ball milling 6 hours, discharging post-drying, crosses 40 mesh sieves;It is subsequently adding the paraffin that percentage by weight is 8% Carry out granulation as adhesive, and cross 80 mesh sieves;It is pressed into a diameter of 10mm with the pressure of 2MPa again with powder compressing machine, Thickness is the base substrate of 5mm;
5. by base substrate in 850 DEG C of sintering, it is incubated 4 hours, prepares low-temperature sintering low-loss microwave-medium Li3Mg2NbO6Pottery Porcelain;
Finally, gained sample microwave property is tested by Network Analyzer and dependence test fixture.
Embodiment 5:
1. according to microwave-medium ceramics component Li3Mg2NbO6, claim Li2CO3-6.8344g、MgO-4.9705g、Nb2O5- -8.1951g dispensing, altogether 20g;Mixed powder adds in polyester tank, after adding 160ml deionized water and 150g zirconium ball, Ball milling 6 hours on planetary ball mill, drum's speed of rotation is 1000 revs/min;
2. the raw material after ball milling is placed in drying box, dries in 120 DEG C and cross 40 mesh sieves, it is thus achieved that evengranular powder;
3. powder is calcined 4 hours in 1050 DEG C;
4. the powder after calcining is put in polyester tank, then after weighing ZBS-0.6000g that mass fraction is 3.0% and calcining Powder mixing, secondary ball milling 6 hours, discharging post-drying, cross 40 mesh sieves;It is subsequently adding the stone that percentage by weight is 8% Wax carries out granulation as adhesive, and crosses 80 mesh sieves;It is pressed into a diameter of 10mm with the pressure of 2MPa again with powder compressing machine, Thickness is the base substrate of 5mm;
5. by base substrate in 850 DEG C of sintering, it is incubated 4 hours, prepares low-temperature sintering low-loss microwave-medium Li3Mg2NbO6Pottery Porcelain;
Finally, gained sample microwave property is tested by Network Analyzer and dependence test fixture.
Embodiment 6:
1. according to microwave-medium ceramics component Li3Mg2NbO6, claim Li2CO3-6.8344g、MgO-4.9705g、Nb2O5- -8.1951g dispensing, altogether 20g;Mixed powder adds in polyester tank, after adding 160ml deionized water and 150g zirconium ball, Ball milling 6 hours on planetary ball mill, drum's speed of rotation is 1000 revs/min;
2. the raw material after ball milling is placed in drying box, dries in 120 DEG C and cross 40 mesh sieves, it is thus achieved that evengranular powder;
3. powder is calcined 4 hours in 1050 DEG C;
4. the powder after calcining is put in polyester tank, then after weighing ZBS-0.0200g that mass fraction is 0.1% and calcining Powder mixing, secondary ball milling 6 hours, discharging post-drying, cross 40 mesh sieves;It is subsequently adding the stone that percentage by weight is 8% Wax carries out granulation as adhesive, and crosses 80 mesh sieves;It is pressed into a diameter of 10mm with the pressure of 2MPa again with powder compressing machine, Thickness is the base substrate of 5mm;
5. by base substrate in 875 DEG C of sintering, it is incubated 4 hours, prepares low-temperature sintering low-loss microwave-medium Li3Mg2NbO6Pottery Porcelain;
Finally, gained sample microwave property is tested by Network Analyzer and dependence test fixture.
Embodiment 7:
1. according to microwave-medium ceramics component Li3Mg2NbO6, claim Li2CO3-6.8344g、MgO-4.9705g、Nb2O5- -8.1951g dispensing, altogether 20g;Mixed powder adds in polyester tank, after adding 160ml deionized water and 150g zirconium ball, Ball milling 6 hours on planetary ball mill, drum's speed of rotation is 1000 revs/min;
2. the raw material after ball milling is placed in drying box, dries in 120 DEG C and cross 40 mesh sieves, it is thus achieved that evengranular powder;
3. powder is calcined 4 hours in 1050 DEG C;
4. the powder after calcining is put in polyester tank, then after weighing ZBS-0.1000g that mass fraction is 0.5% and calcining Powder mixing, secondary ball milling 6 hours, discharging post-drying, cross 40 mesh sieves;It is subsequently adding the stone that percentage by weight is 8% Wax carries out granulation as adhesive, and crosses 80 mesh sieves;It is pressed into a diameter of 10mm with the pressure of 2MPa again with powder compressing machine, Thickness is the base substrate of 5mm;
5. by base substrate in 875 DEG C of sintering, it is incubated 4 hours, prepares low-temperature sintering low-loss microwave-medium Li3Mg2NbO6Pottery Porcelain;
Finally, gained sample microwave property is tested by Network Analyzer and dependence test fixture.
Embodiment 8:
1. according to microwave-medium ceramics component Li3Mg2NbO6, claim Li2CO3-6.8344g、MgO-4.9705g、Nb2O5- -8.1951g dispensing, altogether 20g;Mixed powder adds in polyester tank, after adding 160ml deionized water and 150g zirconium ball, Ball milling 6 hours on planetary ball mill, drum's speed of rotation is 1000 revs/min;
2. the raw material after ball milling is placed in drying box, dries in 120 DEG C and cross 40 mesh sieves, it is thus achieved that evengranular powder;
3. powder is calcined 4 hours in 1050 DEG C;
4. the powder after calcining is put in polyester tank, then after weighing ZBS-0.2000g that mass fraction is 1% and calcining Powder mixes, secondary ball milling 6 hours, discharging post-drying, crosses 40 mesh sieves;It is subsequently adding the paraffin that percentage by weight is 8% Carry out granulation as adhesive, and cross 80 mesh sieves;It is pressed into a diameter of 10mm with the pressure of 2MPa again with powder compressing machine, Thickness is the base substrate of 5mm;
5. by base substrate in 875 DEG C of sintering, it is incubated 4 hours, prepares low-temperature sintering low-loss microwave-medium Li3Mg2NbO6Pottery Porcelain;
Finally, gained sample microwave property is tested by Network Analyzer and dependence test fixture.
Embodiment 9:
1. according to microwave-medium ceramics component Li3Mg2NbO6, claim Li2CO3-6.8344g、MgO-4.9705g、Nb2O5- -8.1951g dispensing, altogether 20g;Mixed powder adds in polyester tank, after adding 160ml deionized water and 150g zirconium ball, Ball milling 6 hours on planetary ball mill, drum's speed of rotation is 1000 revs/min;
2. the raw material after ball milling is placed in drying box, dries in 120 DEG C and cross 40 mesh sieves, it is thus achieved that evengranular powder;
3. powder is calcined 4 hours in 1050 DEG C;
4. the powder after calcining is put in polyester tank, then after weighing ZBS-0.4000g that mass fraction is 2% and calcining Powder mixes, secondary ball milling 6 hours, discharging post-drying, crosses 40 mesh sieves;It is subsequently adding the paraffin that percentage by weight is 8% Carry out granulation as adhesive, and cross 80 mesh sieves;It is pressed into a diameter of 10mm with the pressure of 2MPa again with powder compressing machine, Thickness is the base substrate of 5mm;
5. by base substrate in 875 DEG C of sintering, it is incubated 4 hours, prepares low-temperature sintering low-loss microwave-medium Li3Mg2NbO6Pottery Porcelain;
Finally, gained sample microwave property is tested by Network Analyzer and dependence test fixture.
Embodiment 10:
1. according to microwave-medium ceramics component Li3Mg2NbO6, claim Li2CO3-6.8344g、MgO-4.9705g、Nb2O5- -8.1951g dispensing, altogether 20g;Mixed powder adds in polyester tank, after adding 160ml deionized water and 150g zirconium ball, Ball milling 6 hours on planetary ball mill, drum's speed of rotation is 1000 revs/min;
2. the raw material after ball milling is placed in drying box, dries in 120 DEG C and cross 40 mesh sieves, it is thus achieved that evengranular powder;
3. powder is calcined 4 hours in 1050 DEG C;
4. the powder after calcining is put in polyester tank, then after weighing ZBS-0.6000g that mass fraction is 3.0% and calcining Powder mixing, secondary ball milling 6 hours, discharging post-drying, cross 40 mesh sieves;It is subsequently adding the stone that percentage by weight is 8% Wax carries out granulation as adhesive, and crosses 80 mesh sieves;It is pressed into a diameter of 10mm with the pressure of 2MPa again with powder compressing machine, Thickness is the base substrate of 5mm;
5. by base substrate in 875 DEG C of sintering, it is incubated 4 hours, prepares low-temperature sintering low-loss microwave-medium Li3Mg2NbO6Pottery Porcelain;
Finally, gained sample microwave property is tested by Network Analyzer and dependence test fixture.
Embodiment 11:
1. according to microwave-medium ceramics component Li3Mg2NbO6, claim Li2CO3-6.8344g、MgO-4.9705g、Nb2O5- -8.1951g dispensing, altogether 20g;Mixed powder adds in polyester tank, after adding 160ml deionized water and 150g zirconium ball, Ball milling 6 hours on planetary ball mill, drum's speed of rotation is 1000 revs/min;
2. the raw material after ball milling is placed in drying box, dries in 120 DEG C and cross 40 mesh sieves, it is thus achieved that evengranular powder;
3. powder is calcined 4 hours in 1050 DEG C;
4. the powder after calcining is put in polyester tank, then after weighing ZBS-0.0200g that mass fraction is 0.1% and calcining Powder mixing, secondary ball milling 6 hours, discharging post-drying, cross 40 mesh sieves;It is subsequently adding the stone that percentage by weight is 8% Wax carries out granulation as adhesive, and crosses 80 mesh sieves;It is pressed into a diameter of 10mm with the pressure of 2MPa again with powder compressing machine, Thickness is the base substrate of 5mm;
5. by base substrate in 900 DEG C of sintering, it is incubated 4 hours, prepares low-temperature sintering low-loss microwave-medium Li3Mg2NbO6Pottery Porcelain;
Finally, gained sample microwave property is tested by Network Analyzer and dependence test fixture.
Embodiment 12:
1. according to microwave-medium ceramics component Li3Mg2NbO6, claim Li2CO3-6.8344g、MgO-4.9705g、Nb2O5- -8.1951g dispensing, altogether 20g;Mixed powder adds in polyester tank, after adding 160ml deionized water and 150g zirconium ball, Ball milling 6 hours on planetary ball mill, drum's speed of rotation is 1000 revs/min;
2. the raw material after ball milling is placed in drying box, dries in 120 DEG C and cross 40 mesh sieves, it is thus achieved that evengranular powder;
3. powder is calcined 4 hours in 1050 DEG C;
4. the powder after calcining is put in polyester tank, then after weighing ZBS-0.1000g that mass fraction is 0.5% and calcining Powder mixing, secondary ball milling 6 hours, discharging post-drying, cross 40 mesh sieves;It is subsequently adding the stone that percentage by weight is 8% Wax carries out granulation as adhesive, and crosses 80 mesh sieves;It is pressed into a diameter of 10mm with the pressure of 2MPa again with powder compressing machine, Thickness is the base substrate of 5mm;
5. by base substrate in 900 DEG C of sintering, it is incubated 4 hours, prepares low-temperature sintering low-loss microwave-medium Li3Mg2NbO6Pottery Porcelain;
Finally, gained sample microwave property is tested by Network Analyzer and dependence test fixture.
Embodiment 13:
1. according to microwave-medium ceramics component Li3Mg2NbO6, claim Li2CO3-6.8344g、MgO-4.9705g、Nb2O5- -8.1951g dispensing, altogether 20g;Mixed powder adds in polyester tank, after adding 160ml deionized water and 150g zirconium ball, Ball milling 6 hours on planetary ball mill, drum's speed of rotation is 1000 revs/min;
2. the raw material after ball milling is placed in drying box, dries in 120 DEG C and cross 40 mesh sieves, it is thus achieved that evengranular powder;
3. powder is calcined 4 hours in 1050 DEG C;
4. the powder after calcining is put in polyester tank, then after weighing ZBS-0.2000g that mass fraction is 1% and calcining Powder mixes, secondary ball milling 6 hours, discharging post-drying, crosses 40 mesh sieves;It is subsequently adding the paraffin that percentage by weight is 8% Carry out granulation as adhesive, and cross 80 mesh sieves;It is pressed into a diameter of 10mm with the pressure of 2MPa again with powder compressing machine, Thickness is the base substrate of 5mm;
5. by base substrate in 900 DEG C of sintering, it is incubated 4 hours, prepares low-temperature sintering low-loss microwave-medium Li3Mg2NbO6Pottery Porcelain;
Finally, gained sample microwave property is tested by Network Analyzer and dependence test fixture.
Embodiment 14:
1. according to microwave-medium ceramics component Li3Mg2NbO6, claim Li2CO3-6.8344g、MgO-4.9705g、Nb2O5- -8.1951g dispensing, altogether 20g;Mixed powder adds in polyester tank, after adding 160ml deionized water and 150g zirconium ball, Ball milling 6 hours on planetary ball mill, drum's speed of rotation is 1000 revs/min;
2. the raw material after ball milling is placed in drying box, dries in 120 DEG C and cross 40 mesh sieves, it is thus achieved that evengranular powder;
3. powder is calcined 4 hours in 1050 DEG C;
4. the powder after calcining is put in polyester tank, then after weighing ZBS-0.4000g that mass fraction is 2% and calcining Powder mixes, secondary ball milling 6 hours, discharging post-drying, crosses 40 mesh sieves;It is subsequently adding the paraffin that percentage by weight is 8% Carry out granulation as adhesive, and cross 80 mesh sieves;It is pressed into a diameter of 10mm with the pressure of 2MPa again with powder compressing machine, Thickness is the base substrate of 5mm;
5. by base substrate in 900 DEG C of sintering, it is incubated 4 hours, prepares low-temperature sintering low-loss microwave-medium Li3Mg2NbO6Pottery Porcelain;
Finally, gained sample microwave property is tested by Network Analyzer and dependence test fixture.
Embodiment 15:
1. according to microwave-medium ceramics component Li3Mg2NbO6, claim Li2CO3-6.8344g、MgO-4.9705g、Nb2O5- -8.1951g dispensing, altogether 20g;Mixed powder adds in polyester tank, after adding 160ml deionized water and 150g zirconium ball, Ball milling 6 hours on planetary ball mill, drum's speed of rotation is 1000 revs/min;
2. the raw material after ball milling is placed in drying box, dries in 120 DEG C and cross 40 mesh sieves, it is thus achieved that evengranular powder;
3. powder is calcined 4 hours in 1050 DEG C;
4. the powder after calcining is put in polyester tank, then after weighing ZBS-0.6000g that mass fraction is 3.0% and calcining Powder mixing, secondary ball milling 6 hours, discharging post-drying, cross 40 mesh sieves;It is subsequently adding the stone that percentage by weight is 8% Wax carries out granulation as adhesive, and crosses 80 mesh sieves;It is pressed into a diameter of 10mm with the pressure of 2MPa again with powder compressing machine, Thickness is the base substrate of 5mm;
5. by base substrate in 900 DEG C of sintering, it is incubated 4 hours, prepares low-temperature sintering low-loss microwave-medium Li3Mg2NbO6Pottery Porcelain;
Finally, gained sample microwave property is tested by Network Analyzer and dependence test fixture.
Embodiment 16:
1. according to microwave-medium ceramics component Li3Mg2NbO6, claim Li2CO3-6.8344g、MgO-4.9705g、Nb2O5- -8.1951g dispensing, altogether 20g;Mixed powder adds in polyester tank, after adding 160ml deionized water and 150g zirconium ball, Ball milling 6 hours on planetary ball mill, drum's speed of rotation is 1000 revs/min;
2. the raw material after ball milling is placed in drying box, dries in 120 DEG C and cross 40 mesh sieves, it is thus achieved that evengranular powder;
3. powder is calcined 4 hours in 1050 DEG C;
4. the powder after calcining is put in polyester tank, then after weighing ZBS-0.6000g that mass fraction is 3.0% and calcining Powder mixing, secondary ball milling 6 hours, discharging post-drying, cross 40 mesh sieves;It is subsequently adding the stone that percentage by weight is 8% Wax carries out granulation as adhesive, and crosses 80 mesh sieves;It is pressed into a diameter of 10mm with the pressure of 2MPa again with powder compressing machine, Thickness is the base substrate of 5mm;
5. by base substrate in 925 DEG C of sintering, it is incubated 4 hours, prepares low-temperature sintering low-loss microwave-medium Li3Mg2NbO6Pottery Porcelain;
Finally, gained sample microwave property is tested by Network Analyzer and dependence test fixture.
Embodiment 17:
1. according to microwave-medium ceramics component Li3Mg2NbO6, claim Li2CO3-6.8344g、MgO-4.9705g、Nb2O5- -8.1951g dispensing, altogether 20g;Mixed powder adds in polyester tank, after adding 160ml deionized water and 150g zirconium ball, Ball milling 6 hours on planetary ball mill, drum's speed of rotation is 1000 revs/min;
2. the raw material after ball milling is placed in drying box, dries in 120 DEG C and cross 40 mesh sieves, it is thus achieved that evengranular powder;
3. powder is calcined 4 hours in 1050 DEG C;
4. the powder after calcining is put in polyester tank, then after weighing ZBS-0.0200g that mass fraction is 0.1% and calcining Powder mixing, secondary ball milling 6 hours, discharging post-drying, cross 40 mesh sieves;It is subsequently adding the stone that percentage by weight is 8% Wax carries out granulation as adhesive, and crosses 80 mesh sieves;It is pressed into a diameter of 10mm with the pressure of 2MPa again with powder compressing machine, Thickness is the base substrate of 5mm;
5. by base substrate in 925 DEG C of sintering, it is incubated 4 hours, prepares low-temperature sintering low-loss microwave-medium Li3Mg2NbO6Pottery Porcelain;
Finally, gained sample microwave property is tested by Network Analyzer and dependence test fixture.
Embodiment 18:
1. according to microwave-medium ceramics component Li3Mg2NbO6, claim Li2CO3-6.8344g、MgO-4.9705g、Nb2O5- -8.1951g dispensing, altogether 20g;Mixed powder adds in polyester tank, after adding 160ml deionized water and 150g zirconium ball, Ball milling 6 hours on planetary ball mill, drum's speed of rotation is 1000 revs/min;
2. the raw material after ball milling is placed in drying box, dries in 120 DEG C and cross 40 mesh sieves, it is thus achieved that evengranular powder;
3. powder is calcined 4 hours in 1050 DEG C;
4. the powder after calcining is put in polyester tank, then after weighing ZBS-0.1000g that mass fraction is 0.5% and calcining Powder mixing, secondary ball milling 6 hours, discharging post-drying, cross 40 mesh sieves;It is subsequently adding the stone that percentage by weight is 8% Wax carries out granulation as adhesive, and crosses 80 mesh sieves;It is pressed into a diameter of 10mm with the pressure of 2MPa again with powder compressing machine, Thickness is the base substrate of 5mm;
5. by base substrate in 925 DEG C of sintering, it is incubated 4 hours, prepares low-temperature sintering low-loss microwave-medium Li3Mg2NbO6Pottery Porcelain;
Finally, gained sample microwave property is tested by Network Analyzer and dependence test fixture.
Embodiment 19:
1. according to microwave-medium ceramics component Li3Mg2NbO6, claim Li2CO3-6.8344g、MgO-4.9705g、Nb2O5- -8.1951g dispensing, altogether 20g;Mixed powder adds in polyester tank, after adding 160ml deionized water and 150g zirconium ball, Ball milling 6 hours on planetary ball mill, drum's speed of rotation is 1000 revs/min;
2. the raw material after ball milling is placed in drying box, dries in 120 DEG C and cross 40 mesh sieves, it is thus achieved that evengranular powder;
3. powder is calcined 4 hours in 1050 DEG C;
4. the powder after calcining is put in polyester tank, then after weighing ZBS-0.2000g that mass fraction is 1% and calcining Powder mixes, secondary ball milling 6 hours, discharging post-drying, crosses 40 mesh sieves;It is subsequently adding the paraffin that percentage by weight is 8% Carry out granulation as adhesive, and cross 80 mesh sieves;It is pressed into a diameter of 10mm with the pressure of 2MPa again with powder compressing machine, Thickness is the base substrate of 5mm;
5. by base substrate in 925 DEG C of sintering, it is incubated 4 hours, prepares low-temperature sintering low-loss microwave-medium Li3Mg2NbO6Pottery Porcelain;
Finally, gained sample microwave property is tested by Network Analyzer and dependence test fixture.
Embodiment 20:
1. according to microwave-medium ceramics component Li3Mg2NbO6, claim Li2CO3-6.8344g、MgO-4.9705g、Nb2O5- -8.1951g dispensing, altogether 20g;Mixed powder adds in polyester tank, after adding 160ml deionized water and 150g zirconium ball, Ball milling 6 hours on planetary ball mill, drum's speed of rotation is 1000 revs/min;
2. the raw material after ball milling is placed in drying box, dries in 120 DEG C and cross 40 mesh sieves, it is thus achieved that evengranular powder;
3. powder is calcined 4 hours in 1050 DEG C;
4. the powder after calcining is put in polyester tank, then after weighing ZBS-0.4000g that mass fraction is 2% and calcining Powder mixes, secondary ball milling 6 hours, discharging post-drying, crosses 40 mesh sieves;It is subsequently adding the paraffin that percentage by weight is 8% Carry out granulation as adhesive, and cross 80 mesh sieves;It is pressed into a diameter of 10mm with the pressure of 2MPa again with powder compressing machine, Thickness is the base substrate of 5mm;
5. by base substrate in 925 DEG C of sintering, it is incubated 4 hours, prepares low-temperature sintering low-loss microwave-medium Li3Mg2NbO6Pottery Porcelain;
Finally, gained sample microwave property is tested by Network Analyzer and dependence test fixture.
Embodiment 21:
1. according to microwave-medium ceramics component Li3Mg2NbO6, claim Li2CO3-6.8344g、MgO-4.9705g、Nb2O5- -8.1951g dispensing, altogether 20g;Mixed powder adds in polyester tank, after adding 160ml deionized water and 150g zirconium ball, Ball milling 6 hours on planetary ball mill, drum's speed of rotation is 1000 revs/min;
2. the raw material after ball milling is placed in drying box, dries in 120 DEG C and cross 40 mesh sieves, it is thus achieved that evengranular powder;
3. powder is calcined 4 hours in 1050 DEG C;
4. the powder after calcining is put in polyester tank, then after weighing ZBS-0.6000g that mass fraction is 3.0% and calcining Powder mixing, secondary ball milling 6 hours, discharging post-drying, cross 40 mesh sieves;It is subsequently adding the stone that percentage by weight is 8% Wax carries out granulation as adhesive, and crosses 80 mesh sieves;It is pressed into a diameter of 10mm with the pressure of 2MPa again with powder compressing machine, Thickness is the base substrate of 5mm;
5. by base substrate in 950 DEG C of sintering, it is incubated 4 hours, prepares low-temperature sintering low-loss microwave-medium Li3Mg2NbO6Pottery Porcelain;
Finally, gained sample microwave property is tested by Network Analyzer and dependence test fixture.
Embodiment 22:
1. according to microwave-medium ceramics component Li3Mg2NbO6, claim Li2CO3-6.8344g、MgO-4.9705g、Nb2O5- -8.1951g dispensing, altogether 20g;Mixed powder adds in polyester tank, after adding 160ml deionized water and 150g zirconium ball, Ball milling 6 hours on planetary ball mill, drum's speed of rotation is 1000 revs/min;
2. the raw material after ball milling is placed in drying box, dries in 120 DEG C and cross 40 mesh sieves, it is thus achieved that evengranular powder;
3. powder is calcined 4 hours in 1050 DEG C;
4. the powder after calcining is put in polyester tank, then after weighing ZBS-0.0200g that mass fraction is 0.1% and calcining Powder mixing, secondary ball milling 6 hours, discharging post-drying, cross 40 mesh sieves;It is subsequently adding the stone that percentage by weight is 8% Wax carries out granulation as adhesive, and crosses 80 mesh sieves;It is pressed into a diameter of 10mm with the pressure of 2MPa again with powder compressing machine, Thickness is the base substrate of 5mm;
5. by base substrate in 950 DEG C of sintering, it is incubated 4 hours, prepares low-temperature sintering low-loss microwave-medium Li3Mg2NbO6Pottery Porcelain;
Finally, gained sample microwave property is tested by Network Analyzer and dependence test fixture.
Embodiment 23:
1. according to microwave-medium ceramics component Li3Mg2NbO6, claim Li2CO3-6.8344g、MgO-4.9705g、Nb2O5- -8.1951g dispensing, altogether 20g;Mixed powder adds in polyester tank, after adding 160ml deionized water and 150g zirconium ball, Ball milling 6 hours on planetary ball mill, drum's speed of rotation is 1000 revs/min;
2. the raw material after ball milling is placed in drying box, dries in 120 DEG C and cross 40 mesh sieves, it is thus achieved that evengranular powder;
3. powder is calcined 4 hours in 1050 DEG C;
4. the powder after calcining is put in polyester tank, then after weighing ZBS-0.1000g that mass fraction is 0.5% and calcining Powder mixing, secondary ball milling 6 hours, discharging post-drying, cross 40 mesh sieves;It is subsequently adding the stone that percentage by weight is 8% Wax carries out granulation as adhesive, and crosses 80 mesh sieves;It is pressed into a diameter of 10mm with the pressure of 2MPa again with powder compressing machine, Thickness is the base substrate of 5mm;
5. by base substrate in 950 DEG C of sintering, it is incubated 4 hours, prepares low-temperature sintering low-loss microwave-medium Li3Mg2NbO6Pottery Porcelain;
Finally, gained sample microwave property is tested by Network Analyzer and dependence test fixture.
Embodiment 24:
1. according to microwave-medium ceramics component Li3Mg2NbO6, claim Li2CO3-6.8344g、MgO-4.9705g、Nb2O5- -8.1951g dispensing, altogether 20g;Mixed powder adds in polyester tank, after adding 160ml deionized water and 150g zirconium ball, Ball milling 6 hours on planetary ball mill, drum's speed of rotation is 1000 revs/min;
2. the raw material after ball milling is placed in drying box, dries in 120 DEG C and cross 40 mesh sieves, it is thus achieved that evengranular powder;
3. powder is calcined 4 hours in 1050 DEG C;
4. the powder after calcining is put in polyester tank, then after weighing ZBS-0.2000g that mass fraction is 1% and calcining Powder mixes, secondary ball milling 6 hours, discharging post-drying, crosses 40 mesh sieves;It is subsequently adding the paraffin that percentage by weight is 8% Carry out granulation as adhesive, and cross 80 mesh sieves;It is pressed into a diameter of 10mm with the pressure of 2MPa again with powder compressing machine, Thickness is the base substrate of 5mm;
5. by base substrate in 950 DEG C of sintering, it is incubated 4 hours, prepares low-temperature sintering low-loss microwave-medium Li3Mg2NbO6Pottery Porcelain;
Finally, gained sample microwave property is tested by Network Analyzer and dependence test fixture.
Embodiment 25:
1. according to microwave-medium ceramics component Li3Mg2NbO6, claim Li2CO3-6.8344g、MgO-4.9705g、Nb2O5- -8.1951g dispensing, altogether 20g;Mixed powder adds in polyester tank, after adding 160ml deionized water and 150g zirconium ball, Ball milling 6 hours on planetary ball mill, drum's speed of rotation is 1000 revs/min;
2. the raw material after ball milling is placed in drying box, dries in 120 DEG C and cross 40 mesh sieves, it is thus achieved that evengranular powder;
3. powder is calcined 4 hours in 1050 DEG C;
4. the powder after calcining is put in polyester tank, then after weighing ZBS-0.4000g that mass fraction is 2% and calcining Powder mixes, secondary ball milling 6 hours, discharging post-drying, crosses 40 mesh sieves;It is subsequently adding the paraffin that percentage by weight is 8% Carry out granulation as adhesive, and cross 80 mesh sieves;It is pressed into a diameter of 10mm with the pressure of 2MPa again with powder compressing machine, Thickness is the base substrate of 5mm;
5. by base substrate in 950 DEG C of sintering, it is incubated 4 hours, prepares low-temperature sintering low-loss microwave-medium Li3Mg2NbO6Pottery Porcelain;
Finally, gained sample microwave property is tested by Network Analyzer and dependence test fixture.
Every key parameter and the dielectric properties testing result of the specific embodiment of the invention refer to table 1.
Table 1
The detection method of the embodiment of the present invention is as follows:
1. diameter and the thickness of sample uses micrometer to measure.
2., by Agilent 8720ES Network Analyzer, use and start to rob the prepared cylindrical ceramic material of parallel plate method measurement Dielectric constant, test fixture is put into ESPEC MC-710F type high/low temperature circulation incubator carry out temperature coefficient of resonance frequency Measurement, temperature range be 25-85 DEG C test frequency in the range of 7-13GHz.
3. use enclosed cell method to measure the quality factor of prepared cylindrical ceramic sample.
The present invention is not limited to above-described embodiment, and the change of a lot of details is possible, but the most therefore this run counter to the present invention's Scope and spirit.

Claims (5)

1. a low-temperature sintering low-loss lithium magnesium niobium series microwave dielectric ceramic, its chemical formula is Li3Mg2NbO6, basis at this The ZBS sintering aid of upper additional 0.5%~3%;
Described ZBS sintering aid is 60wt%ZnO 30wt%B2O310wt%SiO2
The preparation method of this low-temperature sintering low-loss lithium magnesium niobium series microwave dielectric ceramic, has following steps:
(1) with Li2CO3、MgO、Nb2O5For raw material, by Li3Mg2NbO6Stoichiometric proportion carry out weigh dispensing, press Raw material: deionized water: the ratio of abrading-ball=2:16:15 adds in polyester tank, ball milling 6 hours on ball mill;
(2) raw material after step (1) ball milling is put in baking oven, dries at 120 DEG C, grind and then cross 40 mesh sieves, it is thus achieved that Evengranular powder;
(3) powder that step (2) mixes is placed in crucible in 1050 DEG C of calcinings, is incubated 4 hours;
(4) ceramic powder after step (3) is calcined is put in polyester tank, and additional mass percent is the ZBS of 0.5%~3%, It is subsequently adding deionized water and zirconia ball, ball milling 6 hours on ball mill;After drying in ceramic powder additional quality hundred Proportion by subtraction be 8% paraffin carry out granulation as adhesive, cross 80 mesh sieves, then be shaped to base substrate with powder compressing machine;
(5) by step (4) in base substrate at 850~950 DEG C of sintering, be incubated 4 hours, heating rate is 5 DEG C/min, prepare Low-temperature sintering low-loss Li3Mg2NbO6Series microwave dielectric ceramic.
A kind of low-temperature sintering low-loss lithium magnesium niobium series microwave dielectric ceramic the most according to claim 1, it is characterised in that The Li of described step (1)2CO3、MgO、Nb2O5The quality purity of raw material is more than 99.9%.
A kind of low-temperature sintering low-loss lithium magnesium niobium series microwave dielectric ceramic the most according to claim 1, it is characterised in that The mass percent of the additional ZBS of described step (4) is 1.0%.
A kind of low-temperature sintering low-loss lithium magnesium niobium series microwave dielectric ceramic the most according to claim 1, it is characterised in that The operating pressure of the tablet press machine of described step (4) is 2MPa, and base substrate specification is the cylinder of Φ 10mm × 5mm.
A kind of low-temperature sintering low-loss lithium magnesium niobium series microwave dielectric ceramic the most according to claim 1, it is characterised in that The sintering temperature of described step (5) is 925 DEG C.
CN201610414620.9A 2016-06-13 2016-06-13 Low-temperature sintering low-loss magnesium-lithium-niobate-series microwave dielectric ceramic Pending CN105859289A (en)

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CN108147809A (en) * 2018-02-06 2018-06-12 北京元六鸿远电子科技股份有限公司 Low temperature sintering barium-titanium series microwave dielectric material and preparation method
CN109354491A (en) * 2018-09-19 2019-02-19 福建火炬电子科技股份有限公司 A kind of high voltage temperature-stable dielectric material formula and preparation method thereof
CN111943671A (en) * 2020-08-18 2020-11-17 西安邮电大学 Wide-sintering temperature zone low-loss microwave dielectric ceramic and preparation method thereof
CN115894022A (en) * 2022-12-16 2023-04-04 西安邮电大学 Low-temperature sintered high-Q x f-value oxyfluoride microwave dielectric ceramic and preparation method thereof

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CN104140260A (en) * 2014-07-28 2014-11-12 天津大学 Low-temperature sintering method of lithium-magnesium-titanium microwave dielectric ceramic
CN105254299A (en) * 2015-11-03 2016-01-20 天津大学 Low-temperature sintered magnesium lithium niobate system microwave dielectric ceramic
CN105347795A (en) * 2015-10-30 2016-02-24 天津大学 High-quality factor lithium-magnesium-niobium-series microwave dielectric ceramic

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CN104140260A (en) * 2014-07-28 2014-11-12 天津大学 Low-temperature sintering method of lithium-magnesium-titanium microwave dielectric ceramic
CN105347795A (en) * 2015-10-30 2016-02-24 天津大学 High-quality factor lithium-magnesium-niobium-series microwave dielectric ceramic
CN105254299A (en) * 2015-11-03 2016-01-20 天津大学 Low-temperature sintered magnesium lithium niobate system microwave dielectric ceramic

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108147809A (en) * 2018-02-06 2018-06-12 北京元六鸿远电子科技股份有限公司 Low temperature sintering barium-titanium series microwave dielectric material and preparation method
CN109354491A (en) * 2018-09-19 2019-02-19 福建火炬电子科技股份有限公司 A kind of high voltage temperature-stable dielectric material formula and preparation method thereof
CN109354491B (en) * 2018-09-19 2021-07-02 福建火炬电子科技股份有限公司 Formula and preparation method of high-pressure-resistant temperature-stable dielectric material
CN111943671A (en) * 2020-08-18 2020-11-17 西安邮电大学 Wide-sintering temperature zone low-loss microwave dielectric ceramic and preparation method thereof
CN115894022A (en) * 2022-12-16 2023-04-04 西安邮电大学 Low-temperature sintered high-Q x f-value oxyfluoride microwave dielectric ceramic and preparation method thereof
CN115894022B (en) * 2022-12-16 2023-07-14 西安邮电大学 Low-temperature sintered high Q multiplied by f value oxyfluoride microwave dielectric ceramic and preparation method thereof

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