CN102584234A - Environment-friendly low-temperature sintered high-epsilon microwave dielectric ceramic and preparation method thereof - Google Patents

Environment-friendly low-temperature sintered high-epsilon microwave dielectric ceramic and preparation method thereof Download PDF

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CN102584234A
CN102584234A CN2012100643401A CN201210064340A CN102584234A CN 102584234 A CN102584234 A CN 102584234A CN 2012100643401 A CN2012100643401 A CN 2012100643401A CN 201210064340 A CN201210064340 A CN 201210064340A CN 102584234 A CN102584234 A CN 102584234A
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CN102584234B (en
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赵敏
童建喜
许赛卿
唐春宝
黄丹
谭金刚
张斌
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Jiaxing Jiali Electronic Co., Ltd.
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Abstract

The invention discloses an environment-friendly low-temperature sintered high-epsilon microwave dielectric ceramic which has the following formula: Li1+m-nNb1-m-3nTim+4nO3+awt%ZnNb2O6+bwt%MnCO3+cwt%CuO+dwt%Bi2O3+ewt%Li2CO3, wherein m is more than or equal to 0.05 and less than or equal to 0.2, n is more than or equal to 0.05 and less than or equal to 0.175, a is more than or equal to 0 but less than and equal to 10, b is more than or equal to 0 and less than or equal to 4, c is more than 0 and less than or equal to 4, d is more than or equal to 0 and less than or equal to 4, e is more than 0 and less than or equal to 6, and a, b, c, d and e are a mass fraction. In the formula, ZnNb2O3 is added to adjust the frequency temperature coefficient, so that the frequency temperature coefficient of the Li1+m-nNb1-m-3nTim+4nO3 ceramic approaches to zero; and the combined use of MnCO3, CuO, Bi2O3 and Li2O3 which conform to the environmental requirements can reduce the sintering temperature of the Li1+m-nNb1-m-3nTim+4nO3 ceramic to be below 900 DEG C, so as to achieve the effect of co-firing with a high electric conductivity silver electrode and also maintain excellent microwave dielectric property (epsilon is equal to 50 to 75, Qf is more than 4000 GHz). The ceramic material can be applied to manufacture high-pass filters, Baluns, Balun filters and other chip-type multilayer microwave ceramic elements in wireless communication.

Description

A kind of environment-friendly type low-temperature sintering high dielectric microwave media ceramic and preparation method thereof
Technical field
The invention belongs to the microwave-medium ceramics field, relate in particular to a kind of environment-friendly type low temperature sintering high-dielectric constant microwave-medium pottery and preparation method thereof.
Background technology
In recent years; Along with the microelectronics fast development of information technology; The needs of complete electronic set aspect miniaturized, portable, multi-functional, digitizing, high frequencyization and high reliability, high-performance have promoted electronic component and have developed to direction microminiaturized, integrated and high frequencyization.LTCC Low Temperature Co-fired Ceramic (LTCC) technology has realized design requirementss such as device volume is little, compact construction, multifunction, stable performance; Become passive integrated mainstream technology, become the developing direction in passive device field and the point of economic increase of new components and parts industry.In order to satisfy microminiaturized needs; To reduce size of devices as far as possible; Wherein the square root of the size of resonator and specific inductivity is inversely proportional to; Therefore to reduce the size of tank circuit, require specific inductivity to want high, the temperature coefficient of resonance frequency τ that therefore seeks high-k, low-loss and be high-quality-factor Qf value (GHz) and go to zero f, LTCC is people's research focus with microwave-medium ceramics.
Li 2O-Nb 2O 5-TiO 2M-Phase (the Li that system exists 1+m-nNb 1-m-3nTi M+4nO 3) solid solution range has excellent microwave dielectric property (ε r=50 ~ 78, Qf is up to 9000GHz, τ fBut seriation), be a kind of microwave dielectric material of excellent performance.In addition, with BaO-TiO 2, BaO-Nd 2O 3-TiO 2, CaO-Li 2O-Sm 2O 3-TiO 2, CaO-Sm 2O 3-TiO 2(sintering temperature is all 1300 Deng high dielectric constant material ℃More than) compare Li 2O-Nb 2O 5-TiO 2Has lower sintering temperature (about 1100 ℃), through a small amount of doping, can realize low-temperature sintering.
At present both at home and abroad to Li 2O-Nb 2O 5-TiO 2The low-temperature sintering of system material has some research reports, and wherein, patent ZL200910042201.7 discloses through adding V 2O 5, H 3BO 3Or Li 2O and V 2O 5Mixture realize Li 2O-Nb 2O 5-TiO 2The low-temperature sintering of system; Patent ZL200710060654.3 discloses through adding B 2O 3, Bi 2O 3, CuO and Pb 3O 4-SiO 2-Bi 2O 3-ZnO-TiO 2-B 2O 3Glass powder reduces Li 2O-Nb 2O 5-TiO 2The system sintering temperature; " the Effect of Li that DongHeonKang etc. deliver at " S ℃ of iety of Journal of the European Ceramic " 2006 26 volumes 2117-2121 page or leaf 2O-V 2O 5On the low temperature sintering and microwave dielectric properties of Li 1.0Nb 0.6Ti 0.5O 3Ceramics " in the literary composition through adding Li 2O-V 2O 5Realize Li 1.0Nb 0.6Ti 0.5O 3Low temperature burn sintering.About Li 2O-Nb 2O 5-TiO 2In the report of system, reduce its sintering temperature to add low melting point mostly, the cooling auxiliary agent that is added generally includes: V 2O 5, contain Pb glass auxiliary agent, B 2O 3, H 3BO 3Wherein one or more.V wherein 2O 5, the starting material Pb that contains Pb glass has severe toxicity, can not satisfy the environmental protection needs of paying attention to day by day.In addition, B 2O 3And H 3BO 3Reactions such as the tackiness agent during easy and curtain coating is filled a prescription, dispersion agent are difficult for processing casting slurry.Therefore, the low-temperature sintering Li that can be made into casting slurry of preparation environment-friendly type 2O-Nb 2O 5-TiO 2It is particularly important that ceramic powder seems.
Summary of the invention
The objective of the invention is to overcome the shortcoming and defect of prior art; An object of the present invention is to provide a kind of environment-friendly type low-temperature sintering high dielectric microwave media ceramic, this stupalith for can 900 ℃ of dense sinterings, high-k, low-dielectric loss, level off to zero frequency-temperature coefficient, can burn, can be made into microwave dielectric material casting slurry, compliance with environmental protection requirements altogether with electrode in the silver metal of high conductivity.An object of the present invention is to provide the preparation method of above-mentioned stupalith.
In order to realize first above-mentioned purpose, the technical scheme below the present invention has adopted:
A kind of environment-friendly type low-temperature sintering high dielectric microwave media ceramic, its composition formula is:
Li 1+m-nNb 1-m-3nTi m+4nO 3+awt%ZnNb 2O 6+bwt%MnCO 3+cwt%CuO?+dwt%Bi 2O 3+ewt%?Li 2CO 3
Wherein: 0.05≤m≤0.2,0.05≤n≤0.175,0≤a≤10,0≤b≤4,0 c≤4,0≤d≤4,0 e≤6, and a, b, c, d and e are massfraction.
As further improvement, the composition formula of described media ceramic is:
LiNb 0.6Ti 0.5O 3+awt%ZnNb 2O 6?+bwt%?MnCO 3?+cwt%?CuO+dwt%?Bi 2O 3+ewt%?Li 2CO 3
Wherein 0≤a≤8,0.5≤b≤4,0.5≤c≤4,0≤d≤2,0 e≤4, a, b, c, d and e are massfraction.
In order to realize second above-mentioned purpose, the technical scheme below the present invention has adopted:
A kind ofly prepare above-mentioned environment-friendly type low-temperature sintering high dielectric microwave media ceramic, this method comprises the steps:
1. with analytical pure Li 2CO 3, Nb 2O 5, TiO 2Press Li in baking under 120 ~ 140 ℃ after 20 ~ 30 hours 1+m-nNb 1-m-3nTi M+4nO 3The chemical formula weighing; With load weighted powder by powder: industrial spirit: the zirconia ball weight ratio is: 1:1.5 ~ 1.8:5 ~ 7, in horizontal ball mill, mixed 24 ~ 30 hours, the slurry that mixes is after 70 ~ 90 ℃ of oven dry; Pre-burning is 4 ~ 6 hours in 800 ~ 900 ℃ of air atmosphere, synthetic Li 2O-Nb 2O 5-TiO 2Base-material, it is for use that the base-material that pre-burning is good is crossed 40 mesh sieves;
2. with analytical pure ZnO, Nb 2O 5Press ZnNb in baking under 120 ~ 140 ℃ after 20 ~ 30 hours 2O 6The chemical formula weighing; With load weighted powder by powder: industrial spirit: the zirconia ball weight ratio is: 1:1.5 ~ 1.8:5 ~ 7, in horizontal ball mill, mixed 24 ~ 30 hours, the slurry that mixes is after 70 ~ 90 ℃ of oven dry; Pre-burning is 4 ~ 6 hours in 800 ~ 900 ℃ of air atmosphere, synthetic ZnNb 2O 6, the ZnNb that pre-burning is good 2O 6Sieve with 40 eye mesh screens;
3. above-mentioned pre-burning is good Li 2O-Nb 2O 5-TiO 2, ZnNb 2O 6And MnCO 3, CuO, Bi 2O 3, Li 2CO 3By proportioning Li 1+m-nNb 1-m-3nTi M+4nO 3+ awt%ZnNb 2O 6+ bwt%MnCO 3+ cwt%CuO+dwt%Bi 2O 3+ ewt%Li 2CO 3Carry out weighing, with load weighted powder by powder: industrial spirit: the zirconia ball weight ratio is: 1:1.3 ~ 1.6:5 ~ 7, in horizontal ball mill, mixed 18 ~ 24 hours; The slurry that mixes is after 70 ~ 90 ℃ of oven dry; Add the granulation of 5wt% poly (vinyl alcohol) binder, press down at 4 ~ 6MPa pressure and process piece, sintering in 850 ~ 900 ℃ of air atmosphere; Be incubated 2 ~ 4 hours, promptly obtain stupalith of the present invention.
The present invention who adopts above-mentioned prescription and technology to form can obtain ε r=50 ~ 78, Qf>4000GHz, temperature coefficient of resonance frequency τ f~ 0 low-temperature sintering microwave medium pottery, performance index satisfy the design requirements of multi-layer RF components and parts fully.The present invention has following characteristics:
1. add ZnNb in the prescription 2O 6The regulating frequency temperature factor makes Li 2O-Nb 2O 5-TiO 2The frequency-temperature coefficient τ of pottery fLevel off to zero;
2. compound interpolation MnCO 3, CuO, Bi 2O 3, Li 2CO 3, make Li 2O-Nb 2O 5-TiO 2Pottery can be 900 ℃Dense sintering is regulated each auxiliary agent content, can realize the common burning of pottery and Ag inner electrode, satisfies the basic demand of chip multilayer microwave device;
3. the sintering aid compliance with environmental protection requirements that adopts of the present invention;
4. material technology of the present invention is simple, stable, favorable reproducibility;
5. material of the present invention has been applied to produce, can prepare chip multilayer microwave ceramic components such as Hi-pass filter in the cableless communication, Ba Lun, Ba Lun wave filter with this material.
Description of drawings
Fig. 1 is (m=0.1, n=0.1, a=6, b=0.5, c=1, d=0.25, the LiNb that e=2) under 900 ℃ of sintering temperatures, obtains of formula number 5 among the embodiment 0.6Ti 0.5O 3The stereoscan photograph of pottery.
Fig. 2 is for using formula number 4 among the embodiment (m=0.1, n=0.1, a=4, b=1.5, c=1.5, d=0.5, e=2) the Ba Lun wave filter profile photo (50 times of magnifications) processed of material.
Embodiment
Embodiment 1
1. with analytical pure Quilonum Retard (Li 2CO 3), Niobium Pentxoxide (Nb 2O 5), titanium oxide (TiO 2) 130 ℃Under dry by the fire after 24 hours by LiNb 0.6Ti 0.5O 3(be m=0.1, n=0.1) chemical formula weighing, with load weighted powder by powder: industrial spirit: the zirconia ball weight ratio is: 1:1.7:5; In horizontal ball mill, mixed 24 hours; The slurry that mixes is after 80 ℃ of oven dry, and pre-burning is 4 hours in 850 ℃ of air atmosphere, synthetic LiNb 0.6Ti 0.5O 3, the LiNb that pre-burning is good 0.6Ti 0.5O 3Sieve with 40 eye mesh screens.
2. with analytical pure zinc oxide (ZnO), Niobium Pentxoxide (Nb 2O 5) press ZnNb in baking under 130 ℃ after 24 hours 2O 6The chemical formula weighing, with load weighted powder by powder: industrial spirit: the zirconia ball weight ratio is: 1:1.5:5, in horizontal ball mill, mixed 24 hours, the slurry that mixes is after 80 ℃ of oven dry, pre-burning is 4 hours in 800 ℃ of air atmosphere, synthetic ZnNb 2O 6, the ZnNb that pre-burning is good 2O 6Sieve with 40 eye mesh screens.
3. above-mentioned pre-burning is good LiNb 0.6Ti 0.5O 3And ZnNb 2O 6And MnCO 3, CuO, Bi 2O 3, Li 2CO 3Press LiNb 0.6Ti 0.5O 3+ awt%ZnNb 2O 6+ bwt%MnCO 3+ cwt%CuO+dwt%Bi 2O 3+ ewt%Li 2CO 3(concrete prescription see table 1) formed weighing, with load weighted powder by powder: industrial spirit: the zirconia ball weight ratio is: 1:1.5:7, ball mill mixing 24 hours; The slurry that mixes is after 80 ℃ of oven dry; Add the granulation of 5wt% Z 150PH (PVA) tackiness agent, press down at 4 ~ 6MPa pressure that to process diameter be 20mm, thickness is the nahlock of 8 ~ 9mm; Sintering in 900 ℃ of air atmosphere is incubated 3 hours and promptly obtains stupalith of the present invention.
The volume density of nahlock sample records with Archimedes's method behind the sintering, adopts the grain morphology characteristic of Japanese Hitachi S4800 field emission scanning electron microscope (FESEM) observing samples sintering section.Agilent 8719ET is adopted in sample surfaces polishing back, and (50MHz ~ 13.5GHz) network analyzer is surveyed its microwave dielectric property.The frequency-temperature coefficient τ of sample fIn 25 ~ 80 ℃ of TRs, record, and by formula τ f=(f 80-f 25)/(f 25* 55) calculate, wherein f 80And f 25It is respectively the resonance mid-frequency under 80 ℃ and 25 ℃.
Table 1 shows density among the embodiment, microwave dielectric property (test frequency is 3GHz) and component relationship.
Table 1
Numbering m n a b c d e Density (g/cm 3） ε r Qf(GHz) τ f ppm/℃)
1 0.1 0.1 4 0 1.5 1.5 2 4.09 64.29 5340 15
2 0.1 0.1 4 0.5 1 1 2 4.02 64.76 4492 9
3 0.1 0.1 6 1 0.5 1 2 4.03 67.57 4568 8
4 0.1 0.1 4 1.5 1.5 0.5 2 4.10 65.39 4282 9
5 0.1 0.1 6 0.5 1 0.25 2 4.07 66.30 4576 12
Embodiment 2
1. by forming Li 1.095Nb 0.375Ti 0.8O 3(m=0.1 is n=0.175) through the 1. synthetic Li of embodiment 1 step 1.095Nb 0.375Ti 0.8O 3Base-material.
2. by forming ZnNb 2O 6Through the 2. synthetic ZnNb of embodiment 1 step 2O 6
3. will synthesize good Li 1.095Nb 0.375Ti 0.8O 3And ZnNb 2O 6And MnCO 3, CuO, Bi 2O 3, Li 2CO 3Press Li 1.095Nb 0.375Ti 0.8O 3+ awt%ZnNb 2O 6+ bwt%MnCO 3+ cwt%CuO+dwt%Bi 2O 3+ ewt%Li 2CO 3(concrete prescription is seen table 2) 3. is pressed into nahlock through embodiment 1 step, and sintering in 900 ℃ of air atmosphere is incubated 3 hours and promptly obtains stupalith of the present invention.
Performance measurement method is with embodiment 1, test result such as table 2 (test frequency is 3GHz).
Table 2
Numbering m n a b c d e Density (g/cm 3） ε r Qf(GHz) τ f ppm/℃)
6 0.1 0.175 8 0.5 1 1 2 3.96 60.34 7432 11
7 0.1 0.175 10 1.5 1 0.5 2 3.90 59.21 7649 9
Embodiment 3
1. by forming Li 1.025Nb 0.675Ti 0.4O 3(m=0.1 is n=0.075) through the 1. synthetic Li of embodiment 1 step 1.025Nb 0.675Ti 0.4O 3
2. will synthesize good Li 1.025Nb 0.675Ti 0.4O 3And MnCO 3, CuO, Bi 2O 3, Li 2CO 3Press Li 1.025Nb 0.675Ti 0.4O 3+ bwt%MnCO 3+ cwt%CuO+dwt%Bi 2O 3+ ewt%Li 2CO 3(concrete prescription is seen table 3) 3. is pressed into nahlock through embodiment 1 step, and sintering in 900 ℃ of air atmosphere is incubated 3 hours and promptly obtains stupalith of the present invention.
Performance measurement method is with embodiment 1, test result such as table 3 (test frequency is 3GHz).
Table 3
Numbering m n a b c d e Density (g/cm 3） ε r Qf(GHz) τ f(ppm/℃)
8 0.1 0.075 0 1.5 1.5 0 2 4.15 70.15 3965 7
9 0.1 0.075 0 1.5 1 0.25 2 4.14 70.63 3840 8
The foregoing description has been illustrated technical conceive of the present invention and characteristics, can not limit protection scope of the present invention with this.All equivalences that spirit is done according to the present invention change and modify, and all should be encompassed within protection scope of the present invention.

Claims (3)

1. environment-friendly type low-temperature sintering high dielectric microwave media ceramic is characterized in that its composition formula is:
Li 1+m-nNb 1-m-3nTi m+4nO 3+awt%ZnNb 2O 6+bwt%MnCO 3+cwt%CuO?+dwt%Bi 2O 3+ewt%?Li 2CO 3
Wherein: 0.05≤m≤0.2,0.05≤n≤0.175,0≤a≤10,0≤b≤4,0 c≤4,0≤d≤4,0 e≤6, and a, b, c, d and e are massfraction.
2. a kind of environment-friendly type low-temperature sintering high dielectric microwave media ceramic according to claim 1 is characterized in that its composition formula is:
LiNb 0.6Ti 0.5O 3+awt%ZnNb 2O 6?+bwt%?MnCO 3?+cwt%?CuO+dwt%?Bi 2O 3+ewt%?Li 2CO 3
Wherein 0≤a≤8,0.5≤b≤4,0.5≤c≤4,0≤d≤2,0 e≤4, a, b, c, d and e are massfraction.
3. one kind prepares the described environment-friendly type low-temperature sintering of claim 1 high dielectric microwave media ceramic, it is characterized in that this method comprises the steps:
1. with analytical pure Li 2CO 3, Nb 2O 5, TiO 2Press Li in baking under 120 ~ 140 ℃ after 20 ~ 30 hours 1+m-nNb 1-m-3nTi M+4nO 3The chemical formula weighing; With load weighted powder by powder: industrial spirit: the zirconia ball weight ratio is: 1:1.5 ~ 1.8:5 ~ 7, in horizontal ball mill, mixed 24 ~ 30 hours, the slurry that mixes is after 70 ~ 90 ℃ of oven dry; Pre-burning is 4 ~ 6 hours in 800 ~ 900 ℃ of air atmosphere, synthetic Li 2O-Nb 2O 5-TiO 2Base-material, it is for use that the base-material that pre-burning is good is crossed 40 mesh sieves;
2. with analytical pure ZnO, Nb 2O 5Press ZnNb in baking under 120 ~ 140 ℃ after 20 ~ 30 hours 2O 6The chemical formula weighing; With load weighted powder by powder: industrial spirit: the zirconia ball weight ratio is: 1:1.5 ~ 1.8:5 ~ 7, in horizontal ball mill, mixed 24 ~ 30 hours, the slurry that mixes is after 70 ~ 90 ℃ of oven dry; Pre-burning is 4 ~ 6 hours in 800 ~ 900 ℃ of air atmosphere, synthetic ZnNb 2O 6, the ZnNb that pre-burning is good 2O 6Sieve with 40 eye mesh screens;
3. above-mentioned pre-burning is good Li 2O-Nb 2O 5-TiO 2, ZnNb 2O 6And MnCO 3, CuO, Bi 2O 3, Li 2CO 3By proportioning Li 1+m-nNb 1-m-3nTi M+4nO 3+ awt%ZnNb 2O 6+ bwt%MnCO 3+ cwt%CuO+dwt%Bi 2O 3+ ewt%Li 2CO 3Carry out weighing, with load weighted powder by powder: industrial spirit: the zirconia ball weight ratio is: 1:1.3 ~ 1.6:5 ~ 7, in horizontal ball mill, mixed 18 ~ 24 hours; The slurry that mixes is after 70 ~ 90 ℃ of oven dry; Add the granulation of 5wt% poly (vinyl alcohol) binder, press down at 4 ~ 6MPa pressure and process piece, sintering in 850 ~ 900 ℃ of air atmosphere; Be incubated 2 ~ 4 hours, promptly obtain stupalith of the present invention.
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CN104692800A (en) * 2015-02-04 2015-06-10 桂林理工大学 Temperature-stable lead-free giant dielectric constant ceramic material
CN104692800B (en) * 2015-02-04 2016-08-24 桂林理工大学 A kind of temperature-stable unleaded huge dielectric constant ceramic material
CN105693241A (en) * 2016-02-22 2016-06-22 济南大学 High-quality-factor lithium-magnesium-niobium microwave dielectric ceramic and preparation method thereof
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WO2018010633A1 (en) * 2016-07-12 2018-01-18 深圳顺络电子股份有限公司 Cbs-class ltcc material and manufacturing method thereof
US10160689B2 (en) 2016-07-12 2018-12-25 Shenzhen Sunlord Electronics Co., Ltd. CBS-based LTCC material and preparation method thereof
CN106495690A (en) * 2016-10-20 2017-03-15 邓湘凌 Superelevation biology dielectric oxidation zircon ceramic and preparation method thereof
CN108373318A (en) * 2018-05-29 2018-08-07 江西人民输变电有限公司 A kind of processing method of positioning antenna microwave-medium function ceramics
CN112592160A (en) * 2020-12-23 2021-04-02 嘉兴佳利电子有限公司 Complex-phase low-temperature co-fired ceramic material and preparation method thereof
CN112592160B (en) * 2020-12-23 2022-05-24 嘉兴佳利电子有限公司 Complex-phase low-temperature co-fired ceramic material and preparation method thereof
CN114573333A (en) * 2022-02-28 2022-06-03 嘉兴佳利电子有限公司 Low-dielectric wollastonite low-temperature co-fired ceramic material and preparation method thereof

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