CN103435344B - Piezoceramic material for high-frequency ceramic filter - Google Patents
Piezoceramic material for high-frequency ceramic filter Download PDFInfo
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- CN103435344B CN103435344B CN201310349033.2A CN201310349033A CN103435344B CN 103435344 B CN103435344 B CN 103435344B CN 201310349033 A CN201310349033 A CN 201310349033A CN 103435344 B CN103435344 B CN 103435344B
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Abstract
The invention relates to the technical field of inorganic non-metal materials, and in particular relates to a piezoceramic material for a high-frequency ceramic filter. The piezoceramic material comprises the following components: xBa(Sc1/2Nb1/2)O3-mLa(Mg1/2Ti1/2)O3-yPb(Ti0.50Zr0.50)O3, 0.01-0.6wt.% of MnO2, and 0.01-0.6wt.% of LiNbO3, wherein x is greater than or equal to 0.01mol and less than or equal to 0.1mol; m is greater than or equal to 0.01mol and less than or equal to 0.1mol; y is greater than or equal to 0.8mol and less than or equal to 0.98mol; and the sum of x, m and y is equal to 1. The dielectric constant of the prepared piezoceramic material is about 1500, the mechanical quality factor is about 2300, the radial electromechanical coupling coefficient is about 0.70, the temperature coefficient of resonance frequency is less than 0.01% (minus 55 DEG C to +85 DEG C), the time stability of the resonance frequency is good, the change rate is less than 0.005% (when being aged for 200 hours), the medium consumption is less than 0.03%, and the piezoceramic material is good in property stability in the use process and high in security.
Description
Technical field
The present invention relates to technical field of inorganic nonmetallic materials, refer in particular to a kind of Piezoceramic material for high-frequency ceramic filter, it adopts the preparation method of conventional solid phase method pottery, utilize general chemistry raw material, prepare high stable high tension performance piezoelectric ceramic, this piezoelectric ceramic is suitable for preparing high frequency ceramic filter etc.
Technical background
Piezoelectric ceramic has excellent piezoelectric effect, it is the class applied in functional ceramic widely, as transducer, transducer, filter etc., play an important role in national economy and national defense industry, because the piezoelectric property of leadless piezoelectric ceramics and the piezoelectric property of lead zirconate titanate base piezoelectric ceramic differ greatly, at present, the application of piezoelectric ceramic mainly lead zirconate titanate base and ternary thereof and four-component-system piezoelectric ceramics; At present, the temperature stability of lead zirconate titanate base piezoelectric ceramic is poor, along with the change of temperature, the larger drift of easy generation resonance frequency, the larger change of relative bandwidth, resonance frequency time stability is bad, and its rate of change is larger, Qm is lower, is difficult to the requirement meeting high frequency ceramic filter; In order to improve the performance of piezoceramic material, normal adopt two kinds of approach: one is by adding ternary or quaternary to form the object that new material reaches modification in basis material; Two is different on the impact of material property according to different Doped ions, carries out doping vario-property to material; The present invention obtains the niobium scandium acid barium titanium magnesium acid lanthanum zirconium titanium acid lead four-component-system piezoelectric ceramics of High-temperature stabilization high tension performance, can for the preparation of devices such as high frequency ceramic filters; Generally, the sintering temperature of lead titanate piezoelectric ceramics is at 1260 DEG C ~ 1280 DEG C, and the sintering temperature of piezoelectric ceramic of the present invention is 1100-1130 DEG C, reduces energy consumption so greatly, cost-saving, can suppress the volatilization of lead oxide simultaneously.
Summary of the invention
The object of the present invention is achieved like this:
A kind of high frequency ceramic filter piezoelectric ceramic, its formula is: xBa (Sc
1/2nb
1/2) O
3-mLa (Mg
1/2ti
1/2) O
3-yPb (Ti
0.50zr
0.50) O
3+ 0.01 ~ 0.6wt.%MnO
2+ 0.01 ~ 0.6wt.%LiNbO
3; Wherein, 0.01≤x≤0.1 mol, 0.01≤m≤0.1 mol, 0.8≤y≤0.98 mol, x+m+y=1; Wherein Ba (Sc
1/2nb
1/2) O
3, La (Mg
1/2ti
1/2) O
3, Pb (Ti
0.50zr
0.50) O
3, LiNbO
3adopt conventional chemical raw material with Solid phase synthesis respectively.
MnO
2and LiNbO
3addition be (xBa (Sc
1/2nb
1/2) O
3-mLa (Mg
1/2ti
1/2) O
3-y Pb (Ti
0.50zr
0.50) O
3) percentage of quality.
The dielectric constant of described piezoelectric ceramic is 1483-1512, Qm is 2309-2330, radial electromechanical coupling factor is 0.69-0.72, and temperature coefficient of resonance frequency is 0.004%-0.008% in-55 ~+85 DEG C of temperature ranges, the resonance frequency time stability t after aging 200 hours
frfor 0.0035%-0.0047%, dielectric loss is 0.018%-0.028%.
Ba (the Sc that piezoelectric ceramic of the present invention is used
1/2nb
1/2) O
3preparation process comprise: by former for the chemistry of routine
Material BaCO
3and Nb
2o
5and Sc
2o
3by 1:1/4:1/4 molar ratio ingredient, after ground and mixed is even, put into oxidation
In 1250 DEG C of insulations 120 minutes in aluminium crucible, solid state reaction kinetics Ba (Sc
1/2nb
1/2) O
3, grinding after cooling
Cross 200 mesh sieves, for subsequent use.
Piezoelectric ceramic of the present invention La (Mg used
1/2ti
1/2) O
3preparation process comprise: by the chemical raw material of routine
La
2o
3with MgO and TiO
2by 1/2:1/2:1/2 molar ratio ingredient, after ground and mixed is even, put into aluminium oxide
In 1250 DEG C-1270 DEG C insulations 120 minutes in crucible, solid state reaction kinetics La (Mg
1/2ti
1/2) O
3, after cooling
Ground 200 mesh sieves, for subsequent use.
The present invention adopts conventional solid phase method ceramic preparation technique, namely first by formula batching, batch ball mill grinding is mixed, after drying, add adhesive granulation, be pressed into green sheet again, then carry out binder removal and sintering in atmosphere, after insulation also cools naturally, obtain niobium scandium acid barium titanium magnesium acid lanthanum zirconium titanium acid lead four-component-system piezoelectric ceramics, by electrode on pottery, then polarize, aging, survey performance.
The formula of above-mentioned high frequency ceramic filter piezoelectric ceramic preferably adopts following two kinds of schemes:
xBa(Sc
1/2Nb
1/2)O
3-mLa(Mg
1/2Ti
1/2)O
3-yPb(Ti
0.50Zr
0.50)O
3+0.01~0.4wt.%MnO
2+0.01~0.5wt.%
LiNbO
3; Wherein, 0.015≤x≤0.08 mol, 0.015≤m≤0.08 mol, 0.84≤y≤0.97 mol, x+m+y=1.
xBa(Sc
1/2Nb
1/2)O
3-mLa(Mg
1/2Ti
1/2)O
3yPb(Ti
0.50Zr
0.50)O
3+0.01~0.3wt.%MnO
2+0.01~0.4wt.%
LiNbO
3; Wherein, 0.02≤x≤0.06 mol, 0.02≤m≤0.06 mol, 0.88≤y≤0.94 mol, x+m+y=1.
Compared with prior art, tool has the following advantages in the present invention:
The dielectric constant of 1, prepared piezoelectric ceramic is about about 1500, Qm (Q
m) be about 2300, radial electromechanical coupling factor (K
p) be about 0.70, temperature coefficient of resonance frequency (τ
fr) being less than 0.01% (-55 ~+85 DEG C), resonance frequency time stability is good, its rate of change (t
fr) be less than 0.005%(aging 200 hours), dielectric loss (tan δ) is less than 0.03%; In use procedure, stability is good, and fail safe is high.
2, the piezoelectric ceramic performance of this patent is easy to regulate, to meet the requirement of the devices such as series of high-frequency ceramic filter.
3, this pottery adopts conventional solid phase method piezoelectric ceramic preparation technology to be prepared, and the raw material used is conventional chemical raw material, and cost of manufacture is low.The sintering temperature of piezoelectric ceramic of the present invention is 1100-1130 DEG C, reduces energy consumption so greatly, cost-saving, can suppress the volatilization of lead oxide simultaneously.
Embodiment
Now the invention will be further described in conjunction with the embodiments, and table 1 provides the formula of embodiments of the invention totally 4 samples.
The primary raw material of the embodiments of the invention formula of totally 4 samples adopts conventional chemical raw material and pre-synthesis Ba (Sc
1/2nb
1/2) O
3, La (Mg
1/2ti
1/2) O
3, Pb (Ti
0.50zr
0.50) O
3, LiNbO
3prepare burden by above-mentioned formula, the material distilled water prepared or deionized water are adopted the mixing of planetary ball mill ball milling, material: ball: water=1:3:(0.6 ~ 1.0), ball milling is after 4 ~ 8 hours, dry to obtain dry mash, the poly-vinyl alcohol solution that the concentration accounting for its weight 5 ~ 8% is 10% (percentage by weight) is added in dry mash, carry out granulation, mixed rear mistake 40 mesh sieve, under 20 ~ 30Mpa pressure, carry out dry-pressing again become green sheet, then at temperature is 750 ~ 850 DEG C, insulation carries out binder removal in 1 ~ 4 hour, and heating rate is 50 ~ 100 DEG C/h; Then sample is placed in alumina crucible, airtight sintering, sintering temperature is 1100 ~ 1130 DEG C, and temperature retention time is 1 ~ 2 hour, namely obtains potsherd.Potsherd two sides after grinding and polishing is coated to silver electrode, and about 120 DEG C polarization in silicone oil, polarized electric field is 3000 ~ 5000 volts/mm, and the polarization time is 15 ~ 20 minutes; Polarize complete, test resonance frequency, through overaging 200 hours test resonance frequencys, calculates resonance frequency rate (t over time
fr); Polarize complete, through overaging 48 hours, test other performances.
The performance of above-mentioned each formula sample lists in table 2, and as can be seen from Table 2, the dielectric constant (ε) of prepared piezoelectric ceramic is about about 1500, and Qm (Qm) is about 2300, radial electromechanical coupling factor (K
p) be about 0.70, temperature coefficient of resonance frequency (τ
fr) being less than 0.01% (-55-+85 DEG C), resonance frequency time stability is good, its rate of change (t
fr) be less than 0.005%(aging 200 hours), dielectric loss (tan δ) is less than 0.03%.
Table 1 embodiments of the invention are the formula of totally 4 samples and performance
The performance of the table 2 embodiments of the invention formula of totally 4 samples
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (5)
1. a high frequency ceramic filter piezoelectric ceramic, the dielectric constant of described piezoelectric ceramic is 1483-1512, Qm is 2309-2330, radial electromechanical coupling factor is 0.69-0.72, temperature coefficient of resonance frequency is 0.004%-0.008% in-55 ~+85 DEG C of temperature ranges, the resonance frequency time stability t after aging 200 hours
frfor 0.0035%-0.0047%, dielectric loss is 0.018%-0.028%, it is characterized in that: consisting of of described piezoelectric ceramic: xBa (Sc
1/2nb
1/2) O
3-mLa (Mg
1/2ti
1/2) O
3-yPb (Ti
0.50zr
0.50) O
3+ 0.01 ~ 0.6wt.%MnO
2+ 0.01 ~ 0.6wt.%LiNbO
3; Wherein, 0.01≤x≤0.1 mol, 0.01≤m≤0.1 mol, 0.8≤y≤0.98 mol, x+m+y=1; Wherein Ba (Sc
1/2nb
1/2) O
3, La (Mg
1/2ti
1/2) O
3, Pb (Ti
0.50zr
0.50) O
3, LiNbO
3adopt conventional chemical raw material with Solid phase synthesis respectively, MnO
2and LiNbO
3addition be (xBa (Sc
1/2nb
1/2) O
3-mLa (Mg
1/2ti
1/2) O
3-y Pb (Ti
0.50zr
0.50) O
3) quality 0.01 ~ 0.6% and 0.01 ~ 0.6%.
2. a kind of high frequency ceramic filter piezoelectric ceramic as claimed in claim 1, is characterized in that: described Ba (Sc
1/2nb
1/2) O
3preparation process comprise: by the chemical raw material BaCO of routine
3and Nb
2o
5and Sc
2o
3by 1:1/4:1/4 molar ratio ingredient, put into alumina crucible after ground and mixed is even in 1250 DEG C of insulations 120 minutes, solid state reaction kinetics Ba (Sc
1/2nb
1/2) O
3, ground 200 mesh sieves after cooling, for subsequent use.
3. a kind of high frequency ceramic filter piezoelectric ceramic as claimed in claim 1, is characterized in that: described La (Mg
1/2ti
1/2) O
3preparation process comprise: by the chemical raw material La of routine
2o
3with MgO and TiO
2by 1/2:1/2:1/2 molar ratio ingredient, put into alumina crucible after ground and mixed is even in 1250 DEG C-1270 DEG C insulations 120 minutes, solid state reaction kinetics La (Mg
1/2ti
1/2) O
3, ground 200 mesh sieves after cooling, for subsequent use.
4. a kind of high frequency ceramic filter piezoelectric ceramic as claimed in claim 1, is characterized in that: consisting of of described piezoelectric ceramic: xBa (Sc
1/2nb
1/2) O
3-mLa (Mg
1/2ti
1/2) O
3-yPb (Ti
0.50zr
0.50) O
3+ 0.01 ~ 0.4wt.%MnO
2+ 0.01 ~ 0.5wt.%LiNbO
3; Wherein, 0.015≤x≤0.08 mol, 0.015≤m≤0.08 mol, 0.84≤y≤0.97 mol, x+m+y=1.
5. a kind of high frequency ceramic filter piezoelectric ceramic as claimed in claim 1, is characterized in that: consisting of of described piezoelectric ceramic: xBa (Sc
1/2nb
1/2) O
3-mLa (Mg
1/2ti
1/2) O
3-yPb (Ti
0.50zr
0.50) O
3+ 0.01 ~ 0.3wt.%MnO
2+ 0.01 ~ 0.4wt.%LiNbO
3; Wherein, 0.02≤x≤0.06 mol, 0.02≤m≤0.06 mol, 0.88≤y≤0.94 mol, x+m+y=1.
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| CN112645709A (en) * | 2020-12-25 | 2021-04-13 | 湖南瀚德微创医疗科技有限公司 | PZT-based piezoelectric ceramic and preparation method thereof |
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Non-Patent Citations (3)
| Title |
|---|
| LiNbO3基无铅压电陶瓷的研究与进展;赁敦敏等;《功能材料》;20041231;第35卷(第1期);第18-20页 * |
| Morphotropic Phase Diagram and Dielectric and Ferroelectric Properties of (1-x)Ba(Sc1/2Nb1/2)O3-xPbTiO3 Solid Solution;Qian Wei et al.;《Chem. Mater》;20091231;第21卷(第3期);第506-510页 * |
| 微波介质陶瓷的研究进展;刁春丽等;《中国陶瓷》;20100531;第46卷(第5期);第6-9页 * |
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