CN105347795A - High-quality factor lithium-magnesium-niobium-series microwave dielectric ceramic - Google Patents

High-quality factor lithium-magnesium-niobium-series microwave dielectric ceramic Download PDF

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CN105347795A
CN105347795A CN201510728848.0A CN201510728848A CN105347795A CN 105347795 A CN105347795 A CN 105347795A CN 201510728848 A CN201510728848 A CN 201510728848A CN 105347795 A CN105347795 A CN 105347795A
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dielectric ceramic
microwave dielectric
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lithium magnesium
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张平
赵永贵
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Tianjin University
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Tianjin University
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Abstract

The invention discloses high-quality factor lithium-magnesium-niobium-series microwave dielectric ceramic. The ceramic has a chemical formula of Li3(Mg0.95A0.05)2NbO6, wherein A=Ca<2+>, Ni<2+>, Zn<2+> and Mn<2+>. Li2CO3, MgO, CaCO3, NiCO3, ZnO, MnCO3 and Nb2O5 are blended according to the chemical formula, is subjected to ball mill, drying and sieving, the powder is subjected to calcining, secondary ball milling and granulation, the granules are pressed to form a blank, and the blank is sintered at a temperature of 1120-1180 DEG C to form the lithium-magnesium-niobium-series microwave dielectric ceramic. The lithium-magnesium-niobium-series microwave dielectric ceramic has dielectric constant of 12.29-15.62, a quality factor of 52700-96160 GH and a resonant frequency temperature coefficient of -23.08 to -18.47ppm/DEG C, can be prepared by simple and eco-friendly processes and has a use prospect.

Description

A kind of high quality factor lithium magnesium niobium series microwave dielectric ceramic
Technical field
The invention belongs to a kind of take composition as the ceramic composition of feature, particularly a kind of high quality factor lithium magnesium niobium series microwave dielectric ceramic and preparation method thereof.
Background technology
Along with the development of microwave communication techniques, microwave dielectric ceramic materials causes people and more and more pays close attention to, and to have suitable specific inductivity, high quality factor and good temperature coefficient of resonance frequency be three inevitable requirements that microwave dielectric ceramic materials can be applied in microwave device, these three parameters and material to make the size of device, operating frequency and thermostability corresponding.In present application aspect, microwave dielectric ceramic materials is more and more employed in the contour performance microwave device of resonator, wave filter and polyrod antenna, and its effect is more and more important.Therefore anxious pending to functional research of novel microwave dielectric ceramic material.
There is the Li of salt mine structure 3mg 2nbO 6series microwave dielectric ceramic is the Novel microwave dielectric ceramic of just exploitation recently, and it has good microwave dielectric property, and specific inductivity is 16.8, and quality factor are 796430GHz, and temperature coefficient of resonance frequency is-27.2ppm/ DEG C.
But it is at present less to the report of the research of its preparation method and modification.The present invention adopts conventional solid-state method, adopts different divalent-metal ion (Ca 2+, Ni 2+, Zn 2+, Mn 2+) respectively to Li 3mg 2nbO 6in pottery, Mg ion is replaced, ensure on the basis that its specific inductivity remains unchanged substantially, improve more greatly the quality factor of niobic acid neodymium pottery, to a certain degree improve its temperature coefficient of resonance frequency simultaneously, become a kind of desirable microwave dielectric ceramic materials.
Summary of the invention
Object of the present invention is on the basis of existing technology, ensures that its specific inductivity is substantially constant, its quality factor of larger raising, to a certain degree improves its temperature coefficient of resonance frequency simultaneously, provides a kind of with Li 2cO 3, MgO, Nb 2o 5for main raw material, and with appropriate divalent-metal ion (Ca 2+, Ni 2+, Zn 2+, Mn 2+) replace magnesium ion, to prepare the lithium magnesium niobium series microwave dielectric ceramic of high quality factor Q × f.
The present invention is achieved by following technical solution.
1. a high quality factor lithium magnesium niobium series microwave dielectric ceramic, it consists of Li 3(Mg 0.95a 0.05) 2nbO 6, wherein A=Ca 2+, Ni 2+, Zn 2+, Mn 2+;
The preparation method of above-mentioned lithium magnesium niobium series microwave dielectric ceramic, has following steps:
(1) by Li 2cO 3, MgO, CaCO 3, NiCO 3, ZnO, MnCO 3, Nb 2o 5raw material, Li 3(Mg 0.95a 0.05) 2nbO 6prepare burden, wherein A=Ca 2+, Ni 2+, Zn 2+, Mn 2+; In raw material: deionized water: mill ball quality adds in polyester tank than the ratio for 2:16:15, ball milling 6 hours on ball mill;
(2) raw material after step (1) ball milling is placed in loft drier in 120 DEG C of oven dry, crosses 40 mesh sieves after drying, obtain evengranular powder;
(3) powder step (2) mixed was in 1050 DEG C of calcinings 4 hours;
(4) ceramic powder after step (3) being calcined puts into polyester tank, after adding deionized water and zirconia ball, and ball milling 6 hours on ball mill; After oven dry in ceramic powder added weight per-cent be 6 ~ 8% paraffin carry out granulation as tackiness agent, cross 80 mesh sieves, then be shaped to base substrate with powder compressing machine;
(5) just walk the green compact of (4) again in 1120 ~ 1180 DEG C of sintering, be incubated 4 hours, obtained microwave-medium ceramics.
The raw material Li of described step (1) 2cO 3, MgO, CaCO 3, NiCO 3, ZnO, MnCO 3, Nb 2o 5purity be greater than 99%.
Described step (1) and step ball mill are (4) planetary ball mill.
The operating pressure of the tabletting machine of described step (4) is 7MPa.
The green compact specification of described step (4) is the right cylinder of Φ 10mm × 5mm.
The sintering temperature of described step (5) is 1140 DEG C, is incubated 4 hours.
Beneficial effect of the present invention is as follows:
Owing to adopting different divalent-metal ion (Ca 2+, Ni 2+, Zn 2+, Mn 2+) partly replace Li 3mg 2nbO 6middle Mg ion, prepares Li 3(Mg 0.95a 0.05) 2nbO 6(wherein A=Ca 2+, Ni 2+, Zn 2+, Mn 2+) microwave-medium ceramics.When sintering temperature is 1140 DEG C, soaking time 4h, a ball milling, the secondary ball milling time is 6h, and A is Ca 2+during ion, specific inductivity is 15.62, and temperature coefficient of resonance frequency reaches-18.47ppm/ DEG C, and quality factor reach maximum value is 96160GHz.Owing to facilitating the growth of its crystal grain after part ion replacement, decrease its pore, therefore improve quality factor.In addition, this preparation technology is simple, process environmental protection, and preparation is simple, is a kind of up-and-coming microwave dielectric material.
Embodiment
The present invention adopts purity to be greater than the chemical feedstocks Li of 99% 2cO 3, MgO, CaCO 3, NiCO 3, ZnO, MnCO 3, Nb 2o 5prepare novel ceramics as low-loss microwave medium material Li 3mg 2nbO 6.
The present invention is by Li 2cO 3, MgO, CaCO 3, NiCO 3, ZnO, MnCO 3, Nb 2o 5chemical formula Li pressed by raw material 3(Mg 0.95a 0.05) 2nbO 6(wherein A=Ca 2+, Ni 2+, Zn 2+, Mn 2+) prepare burden, materials: 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 infrared drying oven in 120 DEG C of oven dry, crosses 40 mesh sieves, then in 1050 DEG C of calcinings 4 hours; Again the ceramic powder after calcining is put into ball grinder, add zirconia ball and deionized water ball milling 6 hours post-dryings; Again in ceramic powder after the drying added weight per-cent be 6 ~ 8% paraffin wax binder carry out granulation, after crossing 80 mesh sieves, under the pressure of 7MPa, powder being pressed into diameter with powder compressing machine is 10mm, and thickness is the green compact of 5mm; By green compact at 1120 ~ 1180 DEG C of sintering, be incubated 4 hours, obtained lithium magnesium niobium series microwave dielectric ceramic; Finally by the microwave dielectric property of network analyzer test article.
The specific embodiment of the invention is as follows.
Embodiment 1:
1. according to lithium magnesium niobium series microwave dielectric ceramic component Li 3(Mg 0.95a 0.05) 2nbO 6(wherein A=Ca 2+), claim Li 2cO 3-6.7107g, MgO-4.6365g, CaCO 3-0.6060g, Nb 2o 5-8.0468g prepares burden, altogether 20g; Mixed powder adds in polyester tank, after adding 160ml deionized water and 150g zirconium ball, and 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 loft drier, dries in 120 DEG C and cross 40 mesh sieves, obtaining evengranular powder;
3. powder is calcined 4 hours in 1050 DEG C;
4. the powder after calcining is put into polyester tank, secondary ball milling 6 hours, discharging post-drying, cross 40 mesh sieves; Then add weight percent be 6% paraffin carry out granulation as tackiness agent, and cross 80 mesh sieves; Be pressed into diameter for 10mm with powder compressing machine with the pressure of 7MPa again, thickness is the base substrate of 5mm;
5. by base substrate in 1140 DEG C of sintering, be incubated 4 hours, obtained lithium magnesium niobium system Li 3(Mg 0.95ca 0.05) 2nbO 6microwave-medium ceramics;
Finally, by network analyzer test gained sample microwave property.
Embodiment 2:
1. according to lithium magnesium niobium series microwave dielectric ceramic component Li 3(Mg 0.95a 0.05) 2nbO 6(wherein A=Ni 2+), claim Li 2cO 3-6.6731g, MgO-4.6105g, NiCO 3-0.7147g, Nb 2o 5-8.0017g prepares burden, altogether 20g; Mixed powder adds in polyester tank, after adding 160ml deionized water and 150g zirconium ball, and 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 loft drier, dries in 120 DEG C and cross 40 mesh sieves, obtaining evengranular powder;
3. powder is calcined 4 hours in 1050 DEG C;
4. the powder after calcining is put into polyester tank, secondary ball milling 6 hours, discharging post-drying, cross 40 mesh sieves; Then add weight percent be 6% paraffin carry out granulation as tackiness agent, and cross 80 mesh sieves; Be pressed into diameter for 10mm with powder compressing machine with the pressure of 7MPa again, thickness is the base substrate of 5mm;
5. by base substrate in 1140 DEG C of sintering, be incubated 4 hours, obtained lithium magnesium niobium system Li 3(Mg 0.95ni 0.05) 2nbO 6microwave-medium ceramics;
Finally, by network analyzer test gained sample microwave property.
Embodiment 3:
1. according to lithium magnesium niobium series microwave dielectric ceramic component Li 3(Mg 0.95a 0.05) 2nbO 6(wherein A=Zn 2+), claim Li 2cO 3-6.7489g, MgO-4.6629g, ZnO-0.4956g, Nb 2o 5-8.0926g prepares burden, altogether 20g; Mixed powder adds in polyester tank, after adding 160ml deionized water and 150g zirconium ball, and 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 loft drier, dries in 120 DEG C and cross 40 mesh sieves, obtaining evengranular powder;
3. powder is calcined 4 hours in 1050 DEG C;
4. the powder after calcining is put into polyester tank, secondary ball milling 6 hours, discharging post-drying, cross 40 mesh sieves; Then add weight percent be 6% paraffin carry out granulation as tackiness agent, and cross 80 mesh sieves; Be pressed into diameter for 10mm with powder compressing machine with the pressure of 7MPa again, thickness is the base substrate of 5mm;
5. by base substrate in 1140 DEG C of sintering, be incubated 4 hours, obtained lithium magnesium niobium system Li 3(Mg 0.95zn 0.05) 2nbO 6microwave-medium ceramics;
Finally, by network analyzer test gained sample microwave property.
Embodiment 4:
1. according to lithium magnesium niobium series microwave dielectric ceramic component Li 3(Mg 0.95a 0.05) 2nbO 6(wherein A=Mn 2+), claim Li 2cO 3-6.6806g, MgO-4.6157g, MnCO 3-0.6928g, Nb 2o 5-8.00108g prepares burden, altogether 20g; Mixed powder adds in polyester tank, after adding 160ml deionized water and 150g zirconium ball, and 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 loft drier, dries in 120 DEG C and cross 40 mesh sieves, obtaining evengranular powder;
3. powder is calcined 4 hours in 1050 DEG C;
4. the powder after calcining is put into polyester tank, secondary ball milling 6 hours, discharging post-drying, cross 40 mesh sieves; Then add weight percent be 6% paraffin carry out granulation as tackiness agent, and cross 80 mesh sieves; Be pressed into diameter for 10mm with powder compressing machine with the pressure of 7MPa again, thickness is the base substrate of 5mm;
5. by base substrate in 1140 DEG C of sintering, be incubated 4 hours, obtained lithium magnesium niobium system Li 3(Mg 0.95mn 0.05) 2nbO 6microwave-medium ceramics;
Finally, by network analyzer test gained sample microwave property.
Embodiment 5:
1. according to lithium magnesium niobium series microwave dielectric ceramic component Li 3(Mg 0.95a 0.05) 2nbO 6(wherein A=Ca 2+), claim Li 2cO 3-6.7107g, MgO-4.6365g, CaCO 3-0.6060g, Nb 2o 5-8.0468g prepares burden, altogether 20g; Mixed powder adds in polyester tank, after adding 160ml deionized water and 150g zirconium ball, and 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 loft drier, dries in 120 DEG C and cross 40 mesh sieves, obtaining evengranular powder;
3. powder is calcined 4 hours in 1050 DEG C;
4. the powder after calcining is put into polyester tank, secondary ball milling 6 hours, discharging post-drying, cross 40 mesh sieves; Then add weight percent be 6% paraffin carry out granulation as tackiness agent, and cross 80 mesh sieves; Be pressed into diameter for 10mm with powder compressing machine with the pressure of 7MPa again, thickness is the base substrate of 5mm;
5. by base substrate in 1120 DEG C of sintering, be incubated 4 hours, obtained lithium magnesium niobium system Li 3(Mg 0.95ca 0.05) 2nbO 6microwave-medium ceramics;
Finally, by network analyzer test gained sample microwave property.
Embodiment 6:
1. according to lithium magnesium niobium series microwave dielectric ceramic component Li 3(Mg 0.95a 0.05) 2nbO 6(wherein A=Ca 2+), claim Li 2cO 3-6.7107g, MgO-4.6365g, CaCO 3-0.6060g, Nb 2o 5-8.0468g prepares burden, altogether 20g; Mixed powder adds in polyester tank, after adding 160ml deionized water and 150g zirconium ball, and 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 loft drier, dries in 120 DEG C and cross 40 mesh sieves, obtaining evengranular powder;
3. powder is calcined 4 hours in 1050 DEG C;
4. the powder after calcining is put into polyester tank, secondary ball milling 6 hours, discharging post-drying, cross 40 mesh sieves; Then add weight percent be 6% paraffin carry out granulation as tackiness agent, and cross 80 mesh sieves; Be pressed into diameter for 10mm with powder compressing machine with the pressure of 7MPa again, thickness is the base substrate of 5mm;
5. by base substrate in 1160 DEG C of sintering, be incubated 4 hours, obtained lithium magnesium niobium system Li 3(Mg 0.95ca 0.05) 2nbO 6microwave-medium ceramics;
Finally, by network analyzer test gained sample microwave property.
Embodiment 7:
1. according to lithium magnesium niobium series microwave dielectric ceramic component Li 3(Mg 0.95a 0.05) 2nbO 6(wherein A=Ca 2+), claim Li 2cO 3-6.7107g, MgO-4.6365g, CaCO 3-0.6060g, Nb 2o 5-8.0468g prepares burden, altogether 20g; Mixed powder adds in polyester tank, after adding 160ml deionized water and 150g zirconium ball, and 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 loft drier, dries in 120 DEG C and cross 40 mesh sieves, obtaining evengranular powder;
3. powder is calcined 4 hours in 1050 DEG C;
4. the powder after calcining is put into polyester tank, secondary ball milling 6 hours, discharging post-drying, cross 40 mesh sieves; Then add weight percent be 6% paraffin carry out granulation as tackiness agent, and cross 80 mesh sieves; Be pressed into diameter for 10mm with powder compressing machine with the pressure of 7MPa again, thickness is the base substrate of 5mm;
5. by base substrate in 1180 DEG C of sintering, be incubated 4 hours, obtained lithium magnesium niobium system Li 3(Mg 0.95ca 0.05) 2nbO 6microwave-medium ceramics;
Finally, by network analyzer test gained sample microwave property.
Every key parameter of the specific embodiment of the invention and the detected result of dielectric properties thereof refer to table 1.
Table 1
The detection method of the embodiment of the present invention is as follows:
1. the diameter of sample and thickness use milscale to measure.
2. by Agilent8720ES network analyzer, adopt and start to rob the dielectric constant that parallel plate method measures prepared cylindrical ceramic material, test fixture is put into the measurement that ESPECMC-710F type high/low temperature circulation incubator carries out temperature coefficient of resonance frequency, temperature range is that 25-85 DEG C of test frequency is within the scope of 8-12GHz.
3. adopt enclosed cell method to measure the quality factor of prepared cylindrical ceramic sample, test frequency is within the scope of 6-10GHz.
The present invention is not limited to above-described embodiment, and the change of a lot of details is possible, but therefore this do not run counter to scope and spirit of the present invention.

Claims (6)

1. a high quality factor lithium magnesium niobium series microwave dielectric ceramic, it consists of Li 3(Mg 0.95a 0.05) 2nbO 6, wherein A=Ca 2+, Ni 2+, Zn 2+, Mn 2+.
The preparation method of above-mentioned lithium magnesium niobium series microwave dielectric ceramic, has following steps:
(1) by Li 2cO 3, MgO, CaCO 3, NiCO 3, ZnO, MnCO 3, Nb 2o 5raw material, Li 3(Mg 0.95a 0.05) 2nbO 6prepare burden, wherein A=Ca 2+, Ni 2+, Zn 2+, Mn 2+; In raw material: deionized water: mill ball quality adds in polyester tank than the ratio for 2:16:15, ball milling 6 hours on ball mill;
(2) raw material after step (1) ball milling is placed in loft drier in 120 DEG C of oven dry, crosses 40 mesh sieves after drying, obtain evengranular powder;
(3) powder step (2) mixed was in 1050 DEG C of calcinings 4 hours;
(4) ceramic powder after step (3) being calcined puts into polyester tank, after adding deionized water and zirconia ball, and ball milling 6 hours on ball mill; After oven dry in ceramic powder added weight per-cent be 6 ~ 8% paraffin carry out granulation as tackiness agent, cross 80 mesh sieves, then be shaped to base substrate with powder compressing machine;
(5) just walk the green compact of (4) again in 1120 ~ 1180 DEG C of sintering, be incubated 4 hours, obtained microwave-medium ceramics.
2. a kind of low-loss lithium magnesium niobium series microwave dielectric ceramic according to claim 1, is characterized in that, the raw material Li of described step (1) 2cO 3, MgO, CaCO 3, NiCO 3, ZnO, MnCO 3, Nb 2o 5purity be greater than 99%.
3. a kind of low-loss lithium magnesium niobium series microwave dielectric ceramic according to claim 1, it is characterized in that, described step (1) and step ball mill are (4) planetary ball mill.
4. a kind of low-loss lithium magnesium niobium series microwave dielectric ceramic according to claim 1, it is characterized in that, the operating pressure of the tabletting machine of described step (4) is 7MPa.
5. a kind of low-loss lithium magnesium niobium series microwave dielectric ceramic according to claim 1, it is characterized in that, the green compact specification of described step (4) is the right cylinder of Φ 10mm × 5mm.
6. a kind of low-loss lithium magnesium niobium series microwave dielectric ceramic according to claim 1, it is characterized in that, the sintering temperature of described step (5) is 1140 DEG C, is incubated 4 hours.
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Cited By (11)

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CN105859289A (en) * 2016-06-13 2016-08-17 天津大学 Low-temperature sintering low-loss magnesium-lithium-niobate-series microwave dielectric ceramic
CN106083034A (en) * 2016-06-13 2016-11-09 天津大学 A kind of low-loss lithium magnesium titanium series microwave dielectric ceramic
CN106116574A (en) * 2016-06-13 2016-11-16 天津大学 A kind of preparation method of low temperature sintering lithium magnesium niobium series microwave dielectric ceramic
CN106348756A (en) * 2016-10-21 2017-01-25 天津大学 High-Q-value lithium-magnesium-niobium microwave dielectric ceramic
CN106348755A (en) * 2016-10-21 2017-01-25 天津大学 Method of effectively reducing sintering temperature of lithium-magnesium-niobium microwave dielectric ceramics
CN106810209A (en) * 2017-01-12 2017-06-09 天津大学 A kind of high q-factor lithium magnesium titanium series microwave dielectric ceramic
CN106830933A (en) * 2017-01-12 2017-06-13 天津大学 A kind of thermally-stabilised high q-factor lithium magnesium niobium series microwave dielectric ceramic
CN109251028A (en) * 2018-10-26 2019-01-22 天津大学 A kind of low high Q lithium magnesium niobium series microwave dielectric ceramic and preparation method thereof that is situated between
CN111302796A (en) * 2020-02-07 2020-06-19 天津大学 Low-dielectric-coefficient low-loss dielectric material 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
CN112457010A (en) * 2020-12-02 2021-03-09 电子科技大学 Rock salt type reconstructed superlattice structure microwave dielectric ceramic material and preparation method thereof

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105859289A (en) * 2016-06-13 2016-08-17 天津大学 Low-temperature sintering low-loss magnesium-lithium-niobate-series microwave dielectric ceramic
CN106083034A (en) * 2016-06-13 2016-11-09 天津大学 A kind of low-loss lithium magnesium titanium series microwave dielectric ceramic
CN106116574A (en) * 2016-06-13 2016-11-16 天津大学 A kind of preparation method of low temperature sintering lithium magnesium niobium series microwave dielectric ceramic
CN106348756A (en) * 2016-10-21 2017-01-25 天津大学 High-Q-value lithium-magnesium-niobium microwave dielectric ceramic
CN106348755A (en) * 2016-10-21 2017-01-25 天津大学 Method of effectively reducing sintering temperature of lithium-magnesium-niobium microwave dielectric ceramics
CN106810209A (en) * 2017-01-12 2017-06-09 天津大学 A kind of high q-factor lithium magnesium titanium series microwave dielectric ceramic
CN106830933A (en) * 2017-01-12 2017-06-13 天津大学 A kind of thermally-stabilised high q-factor lithium magnesium niobium series microwave dielectric ceramic
CN109251028A (en) * 2018-10-26 2019-01-22 天津大学 A kind of low high Q lithium magnesium niobium series microwave dielectric ceramic and preparation method thereof that is situated between
CN111302796A (en) * 2020-02-07 2020-06-19 天津大学 Low-dielectric-coefficient low-loss dielectric material 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
CN112457010A (en) * 2020-12-02 2021-03-09 电子科技大学 Rock salt type reconstructed superlattice structure microwave dielectric ceramic material and preparation method thereof
CN112457010B (en) * 2020-12-02 2022-03-29 电子科技大学 Rock salt type reconstructed superlattice structure microwave dielectric ceramic material and preparation method thereof

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Application publication date: 20160224