CN1975939A - High-dielectric constant microwave dielectric ceramic and producing method thereof - Google Patents

High-dielectric constant microwave dielectric ceramic and producing method thereof Download PDF

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Publication number
CN1975939A
CN1975939A CN 200610129844 CN200610129844A CN1975939A CN 1975939 A CN1975939 A CN 1975939A CN 200610129844 CN200610129844 CN 200610129844 CN 200610129844 A CN200610129844 A CN 200610129844A CN 1975939 A CN1975939 A CN 1975939A
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hour
raw material
ball milling
medium ceramics
microwave medium
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CN100456393C (en
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李玲霞
赵晶
郭锐
王洪茹
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Tianjin University
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Tianjin University
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Abstract

A method for preparing microwave media ceramic includes applying Ag2O of 40-60 mole%, Nb2O5 of 10-40 mole%, Ta2O5 of 10-40mole%, 1-5wt% of Gd2O3 or 1-5wt% of DY2O3 as raw materials, ball-grinding and sintering said materials to prepare ceramic raw powder of Ag( Nb1 - x Tax )O3 then sintering it at temperature of 1130-1150deg.c for obtaining microwave media ceramic with high dielectric constant.

Description

High-permittivity microwave medium ceramics and preparation method thereof
Technical field
The invention relates to the composition is ceramic composition of feature and preparation method thereof, or rather, is with Ag (Nb about a kind of 1-xTa x) O 3Be ceramic composition of base-material and preparation method thereof.
Background technology
Microwave-medium ceramics is meant and is being used for microwave band (UHF, SHF frequency range) circuit as dielectric material and finish the pottery of one or more functions.Microwave dielectric resonator is widely used in the modern communication device, because compare with traditional metal resonators, it has, and volume is little, in light weight, low cost and other advantages.Along with science and technology development, people have proposed small-sized, portable requirement to communication apparatus.The key of electronics miniaturization is the dielectric constant that effectively increases dielectric material.At present, from point of practical application, the research of the ceramic material of frequency in 0.1～1GHz (as mobile communication) has had and has developed rapidly, and the research of the novel microwave material of high dielectric constant and low dielectric loss becomes the focus of research.
In recent years, the ANT material system has caused people's common concern, this is to have unusual high dielectric constant (ε＞400) because compare it with microwave-medium ceramics system in the past, and the temperature coefficient of capacity of system can be controlled at 0 * 10 by the ratio of Nb in the regulating system and Ta -6℃ -1Near, but the loss of this system is bigger, has greatly influenced its application in practice, so mainly concentrate on the dielectric loss of the reduction system that how to adopt an effective measure for the ANT systematic research." adjustable microwave medium A g (Ta, Nb) O that people such as F.Zimmermann delivered on the 6th phase at Journal of European Ceramic Society in 2004 3Research " in mention Ag (Ta, Nb) O of its preparation 3The dielectric constant of system is 310, and temperature coefficient is adjustable.
Summary of the invention
The purpose of this invention is to provide under a kind of intermediate sintering temperature, the 1MHz test frequency dielectric constant greater than 400, dielectric loss is lower than 10 * 10 -4Ceramic capacitor dielectric material and preparation method thereof.
The present invention is achieved by the following technical programs.
High-permittivity microwave medium ceramics of the present invention, its raw material components and mole percent level are Ag 2O 40-60%, Nb 2O 510-40%, Ta 2O 510-40%, on this basis, the added weight degree is the Gd of 1.0-5.0% 2O 3The perhaps Dy of 1.0-5.0% 2O 3
Preparation method of the present invention has following steps:
(1) by mole degree Nb 2O 510-40%, Ta 2O 510-40% batching, in raw material: deionized water: zirconium ball weight ratio is 1: 1: 1.5 ratio ball milling 3-6 hour;
(2) with the raw material behind the ball milling in 110 ℃～120 ℃ oven dry, again in 1100 ℃～1300 ℃ calcinings, synthetic precursor;
(3) by mole degree Ag 2O40-60%, precursor 40-60% second batch, in raw material: deionized water: zirconium ball weight ratio is 1: 1: 1.5 ratio ball milling 3-6 hour; Pulverize, mix, once more in 110 ℃～120 ℃ oven dry;
(4) raw material after will drying is in 930-970 ℃ of calcining, synthetic frit, and on this basis, adding weight percent content is the Gd of 1.0-5.0% 2O 3The perhaps Dy of 1.0-5.0% 2O 3Again in raw material: deionized water: zirconium ball weight ratio is 1: 1: 1.5 ratio ball milling 6-12 hour, pulverizes, mixes, and ceramic former powder is made in 110 ℃ once more～120 ℃ oven dry;
(5) in the former powder of pottery, add weight ratio be the paraffin of 5-6% as the adhesive granulation, be molded into green compact through the 120-380Mpa single shaft;
(6) with green compact in 1110-1150 ℃ of sintering, be incubated 2-6 hour, make high-permittivity microwave medium ceramics.
(7) gained sample upper and lower surface is applied the silver slurry, prepare electrode through 800 ℃ of-840 ℃ of burning infiltrations;
(8) make the high-frequency dielectric ceramic capacitor behind the welding lead.
The calcination time of step (2) is 3-5 hour.
The calcination time of the synthetic frit of step (4) is 10-12 hour.
The sintering process of step (6) is to be warming up to 550 ℃ through 2-3h, is warming up to 1110-1150 ℃ through 2-3h again.
The present invention can significantly improve the dielectric constant of porcelain simultaneously by adding the dielectric loss that rare earth oxide can reduce the ANT series ceramic material of porcelain effectively.ANT series ceramic material sintering temperature of the present invention low (1110-1150 ℃), and have high-k (ε＞400), low-loss (tg δ＜10 * 10 -4) premium properties, have wide application development prospect.In addition, preparation technology of the present invention is simple, preparation process is pollution-free.
Embodiment
Below in conjunction with embodiment the present invention is further described, but is not limited to embodiment.
The present invention is with analytically pure Nb 2O 5, Ta 2O 5Be raw material, adopt pre-synthetic presoma (Nb xTa 1-x) O 3(x=0.2-0.8), in presoma, add the pure Ag of a certain proportion of analysis again 2O, mixture react under oxidizing atmosphere and generate ANT, add Gd more by a certain percentage 2O 3Perhaps Dy 2O 3
The specific embodiment of the invention is as follows, but is not limited to embodiment.
Embodiment 1:
Take by weighing 12g Nb 2O 5, 12g Ta 2O 5Mixing and ball milling 3h, 110 ℃ of oven dry are fired into frit in 1100 ℃ through 3h again in drying box.Take by weighing 16gAg 2O adds in the above-mentioned frit, makes powder in 930 ℃ of calcinings behind the ball milling 5h, and on this basis, the adding weight percent content is 1.0% Gd 2O 3, dry behind the ball milling 6h.Add 5% paraffin granulation, being pressed into diameter is that 10mm, thickness are the living embryo of circle of 1mm, rises to 550 ℃ through 3h and carry out de-waxing in the high temperature resistance case, is warming up to 1110 ℃ through 2h again, insulation 2h.Gained sample upper and lower surface applies the silver slurry, prepares electrode through 820 ℃ of burning infiltrations; Make the high dielectric microwave ceramic capacitor behind the welding lead.
Embodiment 2:
Take by weighing 12g Nb 2O 5, 12g Ta 2O 5Mixing and ball milling 5h, 110 ℃ of oven dry are fired into frit in 1150 ℃ through 3h again in drying box.Take by weighing 16gAg 2O adds in the above-mentioned frit, makes powder in 950 ℃ of calcinings behind the ball milling 3h, and on this basis, the adding weight percent content is 4.0% Gd 2O 3, dry behind the ball milling 8h.Add 5% paraffin granulation, being pressed into diameter is that 10mm, thickness are the living embryo of circle of 1mm, rises to 550 ℃ through 3h and carry out de-waxing in the high temperature resistance case, is warming up to 1140 ℃ through 2h again, insulation 6h.Gained sample upper and lower surface applies the silver slurry, prepares electrode through 840 ℃ of burning infiltrations; Make the high dielectric microwave ceramic capacitor behind the welding lead.
Embodiment 3:
Take by weighing 10g Nb 2O 5, 16g Ta 2O 5Mixing and ball milling 4h, 120 ℃ of oven dry are fired into frit in 1200 ℃ through 4h again in drying box.Take by weighing 14gAg 2O adds in the above-mentioned frit, makes powder in 960 ℃ of calcinings behind the ball milling 4h, and on this basis, the adding weight percent content is 5.0% Gd 2O 3Dry behind the ball milling 10h.Add 5% paraffin granulation, being pressed into diameter is that 10mm, thickness are the living embryo of circle of 1mm, rises to 550 ℃ through 3h and carry out de-waxing in the high temperature resistance case, is warming up to 1140 ℃ through 2h again, insulation 2h.Gained sample upper and lower surface applies the silver slurry, prepares electrode through 840 ℃ of burning infiltrations; Make the high dielectric microwave ceramic capacitor behind the welding lead.
Embodiment 4:
Take by weighing 10g Nb 2O 5, 16g Ta 2O 5Mixing and ball milling 6h, 120 ℃ of oven dry are fired into frit in 1300 ℃ through 5h again in drying box.Take by weighing 14gAg 2O adds in the above-mentioned frit, makes powder in 930 ℃ of calcinings behind the ball milling 6h, and on this basis, the adding weight percent content is 1.0%Dy 2O 3Dry behind the ball milling 6h.Add 6% paraffin granulation, being pressed into diameter is that 10mm, thickness are the living embryo of circle of 1mm, rises to 550 ℃ through 3h and carry out de-waxing in the high temperature resistance case, is warming up to 1150 ℃ through 2h again, insulation 4h.The upper and lower surface-coated silver of gained sample slurry prepares electrode through 820 ℃ of burning infiltrations; Make the high dielectric microwave ceramic capacitor behind the welding lead.
Embodiment 5:
Take by weighing 12g Nb 2O 5, 12g Ta 2O 5Mixing and ball milling 4h, 120 ℃ of oven dry are fired into frit in 1150 ℃ through 6h again in drying box.Take by weighing 16gAg 2O adds in the above-mentioned frit, makes powder in 940 ℃ of calcinings behind the ball milling 5h, and on this basis, the adding weight percent content is 3.5%Dy 2O 3Dry behind the ball milling 12h.Add 5% paraffin granulation, being pressed into diameter is that 10mm, thickness are the living embryo of circle of 1mm, rises to 550 ℃ through 3h and carry out de-waxing in the high temperature resistance case, is warming up to 1150 ℃ through 2h again, insulation 2h.Gained sample upper and lower surface applies the silver slurry, prepares electrode through 840 ℃ of burning infiltrations; Make the high dielectric microwave ceramic capacitor behind the welding lead.
Embodiment 6:
Take by weighing 12g Nb 2O 5, 12g Ta 2O 5Mixing and ball milling 5h, 120 ℃ of oven dry are fired into frit in 1200 ℃ through 3h again in drying box.Take by weighing 15gAg 2O adds in the above-mentioned frit, makes powder in 960 ℃ of calcinings behind the ball milling 3h, and on this basis, the adding weight percent content is 5.0%Dy 2O 3Dry behind the ball milling 8h.Add 6% paraffin granulation, being pressed into diameter is that 10mm, thickness are the living embryo of circle of 1mm, rises to 550 ℃ through 3h and carry out de-waxing in the high temperature resistance case, is warming up to 1130 ℃ through 2h again, insulation 6h.Gained sample upper and lower surface applies the silver slurry, prepares electrode through 820 ℃ of burning infiltrations; Make the high dielectric microwave ceramic capacitor behind the welding lead.
Method of testing of the present invention is as follows:
One, the detection of the dielectric constant of disc medium
Utilize the capacitance C of HP4278A electric capacity instrument measuring samples, according to the dielectric constant of formula (1) calculation sample.
ϵ = 14.4 × C × d D 2 - - - ( 1 )
Wherein: C is the capacitance of sample, and unit is pF.
D is the diameter of sample, and unit is cm.
D is the thickness of sample, and unit is cm.
Two, the measurement of sample insulation resistivity
Utilize ZC36 type ultra-high resistance instrument to measure the Yang Pinde insulation resistance, utilize following formula to calculate the volume resistivity ρ of material v:
ρ v = R i × π × D 2 4 d ( Ω · cm ) - - - ( 2 )
Wherein: R iBe the insulation resistance of sample, unit is Ω.
D is the diameter of sample, and unit is cm.
D is the thickness of sample, and unit is cm.
Three, the measurement of sample dielectric loss
Utilize the dielectric loss tg δ (1MHz) of HP4278A electric capacity instrument measuring samples.
The test result of the embodiment of the invention is compared with the prior art data such as following table 1.
Table 1
Numbering Sintering temperature (℃) DIELECTRIC CONSTANT (1MHz) Dielectric loss tg δ (1MHz) Insulation resistivity ρ v(Ω·cm)
Embodiment 1 1110 403 8.3×10 -4 ＞10 12
Embodiment 2 1140 578 6.4×10 -4 ＞10 12
Embodiment 3 1140 422 9.8×10 -4 ＞10 12
Embodiment 4 1150 473 10×10 -4 ＞10 12
Embodiment 5 1150 496 7.8×10 -4 ＞10 12
Embodiment 6 1130 453 9.2×10 -4 ＞10 12
Prior art 1150 300-400 18×10 -4 ＞10 11
By the test result of table 1 as can be seen, multiple performance index of the present invention all are better than prior art, and preparation technology is simple, preparation process is pollution-free.
The present invention is described by preferred embodiment, and person skilled obviously can realize the present invention to the suitably change and combination of the techniques described herein scheme under the situation that does not break away from content of the present invention, spirit and scope.The replacement that all are similar and change apparent to those skilled in the artly, they are regarded as being included among spirit of the present invention, scope and the content.

Claims (5)

1. a high-permittivity microwave medium ceramics is characterized in that, its raw material components and mole percent level are Ag 2O40-60%, Nb 2O 510-40%, Ta 2O 510-40%, on this basis, the added weight degree is the Gd of 1.0-5.0% 2O 3The perhaps Dy of 1.0-5.0% 2O 3
2. the preparation method of the high-permittivity microwave medium ceramics of claim 1 is characterized in that, has following steps:
(1) by mole degree Nb 2O 510-40%, Ta 2O 510-40% batching, in raw material: deionized water: zirconium ball weight ratio is 1: 1: 1.5 ratio ball milling 3-6 hour;
(2) with the raw material behind the ball milling in 110 ℃～120 ℃ oven dry, again in 1100 ℃～1300 ℃ calcinings, synthetic precursor;
(3) by mole degree Ag 2O40-60%, precursor 40-60% second batch, in raw material: deionized water: zirconium ball weight ratio is 1: 1: 1.5 ratio ball milling 3-6 hour; Pulverize, mix, once more in 110 ℃～120 ℃ oven dry;
(4) raw material after will drying is in 930-970 ℃ of calcining, synthetic frit, and on this basis, adding weight percent content is the Gd of 1.0-5.0% 2O 3The perhaps Dy of 1.0-5.0% 2O 3Again in raw material: deionized water: zirconium ball weight ratio is 1: 1: 1.5 ratio ball milling 6-12 hour, pulverizes, mixes, and ceramic former powder is made in 110 ℃ once more～120 ℃ oven dry;
(5) in the former powder of pottery, add weight ratio be the paraffin of 5-6% as the adhesive granulation, be molded into green compact through the 120-380Mpa single shaft;
(6) with green compact in 1110-1150 ℃ of sintering, be incubated 2-6 hour, make high-permittivity microwave medium ceramics.
(7) gained sample upper and lower surface is applied the silver slurry, prepare electrode through 800 ℃ of-840 ℃ of burning infiltrations;
(8) make the high-frequency dielectric ceramic capacitor behind the welding lead.
3. according to the preparation method of the described high-permittivity microwave medium ceramics of claim 2, it is characterized in that the calcination time of step (2) is 3-5 hour.
4. according to the preparation method of the described high-permittivity microwave medium ceramics of claim 2, it is characterized in that the calcination time of the synthetic frit of step (4) is 10-12 hour.
5. according to the preparation method of the described high-permittivity microwave medium ceramics of claim 2, it is characterized in that the sintering process of step (6) is to be warming up to 550 ℃ through 2-3h, is warming up to 1110-1150 ℃ through 2-3h again.
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CN104926297A (en) * 2015-06-09 2015-09-23 苏州博恩希普新材料科技有限公司 Microwave dielectric ceramic with stable temperature and adjustable dielectric constant and preparation method
CN105084899A (en) * 2015-09-07 2015-11-25 桂林理工大学 Microwave dielectric ceramic LaYV2O8 with low loss, high thermal stability and ultralow dielectric constant
CN105130434A (en) * 2015-09-08 2015-12-09 桂林理工大学 Dielectric ceramic Pr2YV3O12 with heat stability and ultra low dielectric constant
CN105236976A (en) * 2015-09-28 2016-01-13 中南大学 Microwave dielectric ceramic, preparation method and applications thereof
CN105130435A (en) * 2015-10-07 2015-12-09 桂林理工大学 Temperature stabilization type low-dielectric-constant microwave dielectric ceramic BaLiNd2VO7
CN105294076A (en) * 2015-11-30 2016-02-03 桂林理工大学 High-quality-factor temperature-stable low-dielectric-constant microwave dielectric ceramic LiNbGeO5 and preparation method thereof
CN105601269A (en) * 2016-01-12 2016-05-25 江苏江佳电子股份有限公司 High dielectric constant microwave dielectric ceramic with adjustable dielectric constant and preparation method thereof
CN110105067A (en) * 2019-05-01 2019-08-09 太原师范学院 A kind of high dielectric X7R ceramic medium material and preparation method thereof
CN110105067B (en) * 2019-05-01 2021-12-28 太原师范学院 High-dielectric X7R ceramic dielectric material and preparation method thereof

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