CN102584234B - 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 PDFInfo
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- CN102584234B CN102584234B CN201210064340.1A CN201210064340A CN102584234B CN 102584234 B CN102584234 B CN 102584234B CN 201210064340 A CN201210064340 A CN 201210064340A CN 102584234 B CN102584234 B CN 102584234B
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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
Technical field
The invention belongs to 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, develop rapidly along with microelectronics information technology, the needs of complete electronic set aspect miniaturization, portable, multi-functional, digitizing, high frequency and high reliability, high-performance, have promoted the future development of electronic component to microminiaturized, integrated and high frequency.LTCC Low Temperature Co-fired Ceramic(LTCC) technology has realized the design requirementss such as device volume is little, compact construction, multifunction, stable performance, become the mainstream technology of passive integration, become the developing direction in passive device field and the point of economic increase of new components and parts industry.In order to meet microminiaturized needs, to reduce as far as possible the size of device, wherein the size of resonator and the square root of specific inductivity are 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 finds high-k, low-loss and be high-quality-factor Qf value (GHz) and go to zero
f, LTCC microwave-medium ceramics is people's study hotspot.
Li
2o-Nb
2o
5-TiO
2the M-Phase(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
fcan 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
2deng high dielectric constant material, (sintering temperature is all 1300
℃compare above) Li
2o-Nb
2o
5-TiO
2there is lower sintering temperature (approximately 1100
℃), by 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 by 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 by 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
2system sintering temperature; " the Effect of Li that DongHeonKang etc. deliver at S ℃ of iety > > of < < Journal of the European Ceramic 26 volume 2117-2121 pages in 2006
2o-V
2o
5on the low temperature sintering and microwave dielectric properties of Li
1.0nb
0.6ti
0.5o
3ceramics " in a literary composition by 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 greatly mainly with adding low melting point, the cooling auxiliary agent adding generally includes: V
2o
5, containing Pb glass auxiliary agent, B
2o
3, H
3bO
3wherein one or more.V wherein
2o
5, containing the starting material Pb of Pb glass, have severe toxicity, can not meet the environmental protection needs of increasingly paying attention to.In addition B,
2o
3and H
3bO
3tackiness agent in easily filling a prescription with curtain coating, dispersion agent etc. react, and are difficult for making 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 object 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 sintered high-epsilon microwave dielectric ceramic, this stupalith for can 900 ℃ of dense sinterings, high-k, low-dielectric loss, level off to zero frequency-temperature coefficient, can burn altogether, can be made into microwave dielectric material casting slurry, that meet environmental requirement 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 object, the present invention has adopted following technical scheme:
An environment-friendly type low-temperature sintered high-epsilon microwave dielectric 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, 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
0≤a≤8 wherein, 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 object, the present invention has adopted following technical scheme:
Prepare an above-mentioned environment-friendly type low-temperature sintered high-epsilon microwave dielectric ceramic, the method comprises the following steps:
1. by analytical pure Li
2cO
3, Nb
2o
5, TiO
2at 120 ~ 140 ℃, dry after 20 ~ 30 hours by Li
1+m-nnb
1-m-3nti
m+4no
3chemical formula weighs, by load weighted powder by powder: industrial spirit: zirconia ball weight ratio is: 1:1.5 ~ 1.8:5 ~ 7, in horizontal ball mill, mix 24 ~ 30 hours, the slurry mixing is after 70 ~ 90 ℃ of oven dry, in 800 ~ 900 ℃ of air atmosphere, pre-burning is 4 ~ 6 hours, synthetic Li
2o-Nb
2o
5-TiO
2base-material, it is stand-by that pre-burned base-material is crossed 40 mesh sieves;
2. by analytical pure ZnO, Nb
2o
5at 120 ~ 140 ℃, dry after 20 ~ 30 hours by ZnNb
2o
6chemical formula weighs, by load weighted powder by powder: industrial spirit: zirconia ball weight ratio is: 1:1.5 ~ 1.8:5 ~ 7, in horizontal ball mill, mix 24 ~ 30 hours, the slurry mixing is after 70 ~ 90 ℃ of oven dry, in 800 ~ 900 ℃ of air atmosphere, pre-burning is 4 ~ 6 hours, synthetic ZnNb
2o
6, pre-burned ZnNb
2o
6with 40 eye mesh screens, sieve;
3. by above-mentioned pre-burned 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
3weigh, by load weighted powder by powder: industrial spirit: zirconia ball weight ratio is: 1:1.3 ~ 1.6:5 ~ 7, in horizontal ball mill, mix 18 ~ 24 hours, the slurry mixing is after 70 ~ 90 ℃ of oven dry, add the granulation of 5wt% poly (vinyl alcohol) binder, briquetting under 4 ~ 6MPa pressure, sintering in 850 ~ 900 ℃ of air atmosphere, be incubated 2 ~ 4 hours, obtain stupalith of the present invention.
The present invention who adopts above-mentioned formula and technique to form, can obtain ε r=50 ~ 78, Qf>4000GHz, temperature coefficient of resonance frequency τ
f~ 0 Temperature Firing Microwave Dielectric Ceramics, performance index meet the design requirements of multi-layer RF components and parts completely.The present invention has following characteristics:
1. in formula, add ZnNb
2o
6regulating 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, regulates each auxiliary agent content, can realize the common burning of pottery and Ag inner electrode, meets the basic demand of chip multilayer microwave device;
3. the sintering aid that the present invention adopts meets environmental requirement;
4. simple, stable, the favorable reproducibility of material technology of the present invention;
5. material of the present invention has been applied to produce, can prepare the chip multilayer microwave ceramic components such as Hi-pass filter in cableless communication, Ba Lun, Ba Lun wave filter with this material.
Accompanying drawing explanation
Fig. 1 is formula number 5(m=0.1 in embodiment, n=0.1, a=6, b=0.5, c=1, d=0.25, e=2) LiNb that obtains under 900 ℃ of sintering temperatures
0.6ti
0.5o
3the stereoscan photograph of pottery.
Fig. 2 is for being used formula number 4(m=0.1 in embodiment, 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) made of material.
Embodiment
embodiment 1
1. by analytical pure Quilonum Retard (Li
2cO
3), Niobium Pentxoxide (Nb
2o
5), titanium dioxide (TiO
2) 130
℃lower baking was pressed LiNb after 24 hours
0.6ti
0.5o
3(being m=0.1, n=0.1) chemical formula weighs, by load weighted powder by powder: industrial spirit: zirconia ball weight ratio is: 1:1.7:5, in horizontal ball mill, mix 24 hours, the slurry mixing is after 80 ℃ of oven dry, and in 850 ℃ of air atmosphere, pre-burning is 4 hours, synthetic LiNb
0.6ti
0.5o
3, pre-burned LiNb
0.6ti
0.5o
3with 40 eye mesh screens, sieve.
2. by analytical pure zinc oxide (ZnO), Niobium Pentxoxide (Nb
2o
5) at 130 ℃, dry after 24 hours by ZnNb
2o
6chemical formula weighs, by load weighted powder by powder: industrial spirit: zirconia ball weight ratio is: 1:1.5:5, in horizontal ball mill, mix 24 hours, the slurry mixing is after 80 ℃ of oven dry, in 800 ℃ of air atmosphere, pre-burning is 4 hours, synthesizes ZnNb
2o
6, pre-burned ZnNb
2o
6with 40 eye mesh screens, sieve.
3. by above-mentioned pre-burned 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(specifically filling a prescription in Table 1) forms weighing, by load weighted powder by powder: industrial spirit: zirconia ball weight ratio is: 1:1.5:7, ball milling mixes 24 hours, the slurry mixing is after 80 ℃ of oven dry, add the granulation of 5wt% polyvinyl alcohol (PVA) tackiness agent, under 4 ~ 6MPa pressure, being pressed into diameter is 20mm, the nahlock that thickness is 8 ~ 9mm, sintering in 900 ℃ of air atmosphere, is incubated and within 3 hours, obtains stupalith of the present invention.
After sintering, the volume density of nahlock sample records by Archimedes's method, adopts the grain morphology feature of Japanese Hitachi S4800 field emission scanning electron microscope (FESEM) observing samples sinter section.After sample surfaces polishing, adopting Agilent 8719ET(50MHz ~ 13.5GHz) network analyzer surveys its microwave dielectric property.The frequency-temperature coefficient τ of sample
fin 25 ~ 80 ℃ of temperature ranges, record, and by formula τ
f=(f
80-f
25)/(f
25* 55) calculate, wherein f
80and f
25it is respectively the resonance center frequeH at 80 ℃ and 25 ℃.
Table 1 shows density in 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, n=0.175) 1. synthesizes Li through embodiment 1 step
1.095nb
0.375ti
0.8o
3base-material.
2. by forming ZnNb
2o
6through embodiment 1 step, 2. synthesize ZnNb
2o
6.
3. by synthetic 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(specifically filling a prescription in Table 2) is 3. pressed into nahlock through embodiment 1 step, and sintering in 900 ℃ of air atmosphere is incubated and within 3 hours, obtains stupalith of the present invention.
Performance measurement method is with embodiment 1, and test result is 3GHz as shown 2(test frequency).
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, n=0.075) 1. synthesizes Li through embodiment 1 step
1.025nb
0.675ti
0.4o
3.
2. by synthetic 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(specifically filling a prescription in Table 3) is 3. pressed into nahlock through embodiment 1 step, and sintering in 900 ℃ of air atmosphere is incubated and within 3 hours, obtains stupalith of the present invention.
Performance measurement method is with embodiment 1, and test result is 3GHz as shown 3(test frequency).
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 |
Above-described embodiment has been illustrated technical conceive of the present invention and feature, can not limit the scope of the invention with this.All equivalences that spirit is done according to the present invention change and modify, within all should being encompassed in protection scope of the present invention.
Claims (3)
1. an environment-friendly type low-temperature sintered high-epsilon microwave dielectric 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, a, b, c, d and e are massfraction; Described ceramic preparation method comprises the following steps:
1. by analytical pure Li
2cO
3, Nb
2o
5, TiO
2at 120 ~ 140 ℃, dry after 20 ~ 30 hours by Li
1+m-nnb
1-m-3nti
m+4no
3chemical formula weighs, by load weighted powder by powder: industrial spirit: zirconia ball weight ratio is: 1:1.5 ~ 1.8:5 ~ 7, in horizontal ball mill, mix 24 ~ 30 hours, the slurry mixing is after 70 ~ 90 ℃ of oven dry, in 800 ~ 900 ℃ of air atmosphere, pre-burning is 4 ~ 6 hours, synthetic Li
2o-Nb
2o
5-TiO
2base-material, it is stand-by that pre-burned base-material is crossed 40 mesh sieves;
2. by analytical pure ZnO, Nb
2o
5at 120 ~ 140 ℃, dry after 20 ~ 30 hours by ZnNb
2o
6chemical formula weighs, by load weighted powder by powder: industrial spirit: zirconia ball weight ratio is: 1:1.5 ~ 1.8:5 ~ 7, in horizontal ball mill, mix 24 ~ 30 hours, the slurry mixing is after 70 ~ 90 ℃ of oven dry, in 800 ~ 900 ℃ of air atmosphere, pre-burning is 4 ~ 6 hours, synthetic ZnNb
2o
6, pre-burned ZnNb
2o
6with 40 eye mesh screens, sieve;
3. by above-mentioned pre-burned 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
3weigh, by load weighted powder by powder: industrial spirit: zirconia ball weight ratio is: 1:1.3 ~ 1.6:5 ~ 7, in horizontal ball mill, mix 18 ~ 24 hours, the slurry mixing is after 70 ~ 90 ℃ of oven dry, add the granulation of 5wt% poly (vinyl alcohol) binder, briquetting under 4 ~ 6MPa pressure, sintering in 850 ~ 900 ℃ of air atmosphere, be incubated 2 ~ 4 hours, obtain described stupalith.
2. a kind of environment-friendly type low-temperature sintered high-epsilon microwave dielectric 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
0≤a≤8 wherein, 0.5≤b≤4,0.5≤c≤4,0≤d≤2,0<e≤4, a, b, c, d and e are massfraction.
3. a method of preparing environment-friendly type low-temperature sintered high-epsilon microwave dielectric ceramic claimed in claim 1, is characterized in that the method comprises the following steps:
1. by analytical pure Li
2cO
3, Nb
2o
5, TiO
2at 120 ~ 140 ℃, dry after 20 ~ 30 hours by Li
1+m-nnb
1-m-3nti
m+4no
3chemical formula weighs, by load weighted powder by powder: industrial spirit: zirconia ball weight ratio is: 1:1.5 ~ 1.8:5 ~ 7, in horizontal ball mill, mix 24 ~ 30 hours, the slurry mixing is after 70 ~ 90 ℃ of oven dry, in 800 ~ 900 ℃ of air atmosphere, pre-burning is 4 ~ 6 hours, synthetic Li
2o-Nb
2o
5-TiO
2base-material, it is stand-by that pre-burned base-material is crossed 40 mesh sieves;
2. by analytical pure ZnO, Nb
2o
5at 120 ~ 140 ℃, dry after 20 ~ 30 hours by ZnNb
2o
6chemical formula weighs, by load weighted powder by powder: industrial spirit: zirconia ball weight ratio is: 1:1.5 ~ 1.8:5 ~ 7, in horizontal ball mill, mix 24 ~ 30 hours, the slurry mixing is after 70 ~ 90 ℃ of oven dry, in 800 ~ 900 ℃ of air atmosphere, pre-burning is 4 ~ 6 hours, synthetic ZnNb
2o
6, pre-burned ZnNb
2o
6with 40 eye mesh screens, sieve;
3. by above-mentioned pre-burned 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
3weigh, by load weighted powder by powder: industrial spirit: zirconia ball weight ratio is: 1:1.3 ~ 1.6:5 ~ 7, in horizontal ball mill, mix 18 ~ 24 hours, the slurry mixing is after 70 ~ 90 ℃ of oven dry, add the granulation of 5wt% poly (vinyl alcohol) binder, briquetting under 4 ~ 6MPa pressure, sintering in 850 ~ 900 ℃ of air atmosphere, be incubated 2 ~ 4 hours, obtain described stupalith.
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