CN103435344A - Piezoceramic material for high-frequency ceramic filter - Google Patents
Piezoceramic material for high-frequency ceramic filter Download PDFInfo
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- CN103435344A CN103435344A CN2013103490332A CN201310349033A CN103435344A CN 103435344 A CN103435344 A CN 103435344A CN 2013103490332 A CN2013103490332 A CN 2013103490332A CN 201310349033 A CN201310349033 A CN 201310349033A CN 103435344 A CN103435344 A CN 103435344A
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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 high frequency ceramic filter piezoceramic material, it adopts the preparation method of conventional solid phase method pottery, utilize the general chemistry raw material, prepare high stable high tension performance piezoelectric ceramics, this piezoelectric ceramics is suitable for preparing high frequency ceramic filter etc.
Technical background
Piezoelectric ceramics has good piezoelectric effect, to apply a class very widely in function ceramics, as sensor, transverter, wave filter etc., in national economy and national defense industry, play an important role, because the piezoelectric property of leadless piezoelectric ceramics and the piezoelectric property of Pb-based lanthanumdoped zirconate titanates base piezoelectric ceramic differ greatly, at present, the application of piezoelectric ceramics is mainly Pb-based lanthanumdoped zirconate titanates base and ternary and four-component-system piezoelectric ceramics; At present, the temperature stability of Pb-based lanthanumdoped zirconate titanates base piezoelectric ceramic is poor, variation along with temperature, easily produce the larger drift of resonant frequency, the larger variation of relative bandwidth, the resonant frequency time stability is bad, and its velocity of variation is larger, Qm is lower, is difficult to meet the requirement of high frequency ceramic filter; In order to improve the performance of piezoceramic material, often adopt two kinds of approach: the one, reach the purpose of modification to form novel material by add ternary or quaternary in body material; The 2nd, the difference that affects according to different dopant ions on material property, carry 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 stable high voltage electrical property, can be for the preparation of devices such as high frequency ceramic filters; Generally, the sintering temperature of lead titanate piezoelectric ceramics is at 1260 ℃ ~ 1280 ℃, and the sintering temperature of piezoelectric ceramics of the present invention is 1100-1130 ℃, reduces so greatly energy consumption, cost-saving, simultaneously the volatilization of energy inhibited oxidation lead.
Summary of the invention
The object of the present invention is achieved like this:
A kind of high frequency ceramic filter piezoelectric ceramics, 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; Ba (Sc wherein
1/2nb
1/2) O
3, La (Mg
1/2ti
1/2) O
3, Pb (Ti
0.50zr
0.50) O
3, LiNbO
3respectively to adopt conventional chemical feedstocks synthetic with solid phase method.
MnO
2and LiNbO
3add-on 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) per-cent of quality.
The specific inductivity of described piezoelectric ceramics is 1483-1512, Qm is 2309-2330, radially electromechanical coupling factor is 0.69-0.72, and temperature coefficient of resonance frequency is 0.004%-0.008% in-55 ~+85 ℃ of temperature ranges, the resonant 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 ceramics of the present invention is used
1/2nb
1/2) O
3preparation process comprise: by conventional chemical principle
Material BaCO
3and Nb
2o
5and Sc
2o
3press the 1:1/4:1/4 molar ratio ingredient, after ground and mixed is even, put into oxidation
In the aluminium crucible, in 1250 ℃ of insulations 120 minutes, solid state reaction was synthesized Ba (Sc
1/2nb
1/2) O
3, cooling rear grinding
Cross 200 mesh sieves, standby.
Piezoelectric ceramics of the present invention La (Mg used
1/2ti
1/2) O
3preparation process comprise: by conventional chemical feedstocks
La
2o
3with MgO and TiO
2press the 1/2:1/2:1/2 molar ratio ingredient, after ground and mixed is even, put into aluminum oxide
In crucible, in 1250 ℃-1270 ℃ insulations 120 minutes, solid state reaction was synthesized La (Mg
1/2ti
1/2) O
3, cooling after
Ground 200 mesh sieves, standby.
The present invention adopts conventional solid phase method pottery preparation technology, at first by the formula batching, the admixtion ball mill pulverizing is mixed, after being dried, add the tackiness agent granulation, be pressed into again green sheet, then carry out binder removal and sintering in air, after insulation naturally cooling, obtain niobium scandium acid barium titanium magnesium acid lanthanum zirconium titanium acid lead four-component-system piezoelectric ceramics, on pottery by electrode, then polarization, aging, surveys performance.
Above-mentioned high frequency ceramic filter preferably adopts following two kinds of schemes with the formula of piezoelectric ceramics:
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.
The present invention compared with prior art, has following advantage:
1, the specific inductivity of prepared piezoelectric ceramics is about 1500 left and right, Qm (Q
m) be 2300 left and right, electromechanical coupling factor (K radially
p) be 0.70 left and right, temperature coefficient of resonance frequency (τ
fr) being less than 0.01% (55 ~+85 ℃), the resonant frequency time stability is good, its velocity of variation (t
fr) be less than 0.005%(aging 200 hours), dielectric loss (tan δ) is less than 0.03%; Use procedure performance good stability, safe.
2, the piezoelectric ceramics performance of this patent is easy to regulate, to meet the requirement of the devices such as serial high frequency ceramic filter.
3, this pottery adopts conventional solid phase method piezoelectric ceramics preparation technology to be prepared, and the raw material used is conventional chemical feedstocks, and cost of manufacture is low.The sintering temperature of piezoelectric ceramics of the present invention is 1100-1130 ℃, reduces so greatly energy consumption, cost-saving, simultaneously the volatilization of energy inhibited oxidation lead.
Embodiment
The invention will be further described in conjunction with the embodiments now, and table 1 provides the embodiments of the invention formula of totally 4 samples.
The embodiments of the invention main raw material of the formula of totally 4 samples adopt conventional chemical feedstocks 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
3by above-mentioned formula batching, with distilled water or deionized water, adopt the planetary ball mill ball milling to mix in the material prepared, material: ball: water=1:3:(0.6 ~ 1.0), after ball milling 4 ~ 8 hours, dry to obtain dry mash, add the polyvinyl alcohol solution that the concentration that accounts for its weight 5 ~ 8% is 10% (weight percent) in dry mash, carry out granulation, mixed rear mistake 40 mesh sieves, carrying out dry-pressing again and become green sheet under 20 ~ 30Mpa pressure, is then to be incubated 1 ~ 4 hour under 750 ~ 850 ℃ to carry out binder removal in temperature, and temperature rise rate is 50 ~ 100 ℃/hs; Then sample is placed in to alumina crucible, airtight sintering, sintering temperature is 1100 ~ 1130 ℃, soaking time is 1 ~ 2 hour, obtains ceramic plate.Ceramic plate is two sides coating silver electrode after grinding and polishing, and about 120 ℃ polarization in silicone oil, and polarized electric field is 3000 ~ 5000 volts/mm, and the polarization time is 15 ~ 20 minutes; Polarize complete, the test resonant frequency, through 200 hours test resonant frequencies of overaging, calculate resonant frequency rate (t over time
fr); Polarize complete, through overaging 48 hours, test other performances.
Above-mentioned performance of respectively filling a prescription sample is listed in table 2, and as can be seen from Table 2, the specific inductivity of prepared piezoelectric ceramics (ε) is about 1500 left and right, and Qm (Qm) is 2300 left and right, radially electromechanical coupling factor (K
p) be 0.70 left and right, temperature coefficient of resonance frequency (τ
fr) being less than 0.01% (55-+85 ℃), the resonant frequency time stability is good, its velocity of variation (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 formula and the performance of totally 4 samples
Table 2 embodiments of the invention are the performance of the 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 modifications of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.
Claims (5)
1. a high frequency ceramic filter piezoelectric ceramics, the specific inductivity of described piezoelectric ceramics is 1483-1512, Qm is 2309-2330, radially electromechanical coupling factor is 0.69-0.72, temperature coefficient of resonance frequency is 0.004%-0.008% in-55 ~+85 ℃ of temperature ranges, the resonant 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: the consisting of of described piezoelectric ceramics: 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; Ba (Sc wherein
1/2nb
1/2) O
3, La (Mg
1/2ti
1/2) O
3, Pb (Ti
0.50zr
0.50) O
3, LiNbO
3respectively to adopt conventional chemical feedstocks synthetic with solid phase method, MnO
2and LiNbO
3add-on 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 ceramics as claimed in claim 1, is characterized in that: described Ba (Sc
1/2nb
1/2) O
3preparation process comprise: by conventional chemical feedstocks BaCO
3and Nb
2o
5and Sc
2o
3press the 1:1/4:1/4 molar ratio ingredient, after ground and mixed is even, put into alumina crucible in 1250 ℃ of insulations 120 minutes, solid state reaction is synthesized Ba (Sc
1/2nb
1/2) O
3, ground 200 mesh sieves after cooling, standby.
3. a kind of high frequency ceramic filter piezoelectric ceramics as claimed in claim 1, is characterized in that: described La (Mg
1/2ti
1/2) O
3preparation process comprise: by conventional chemical feedstocks La
2o
3with MgO and TiO
2press the 1/2:1/2:1/2 molar ratio ingredient, after ground and mixed is even, put into alumina crucible in 1250 ℃-1270 ℃ insulations 120 minutes, solid state reaction is synthesized La (Mg
1/2ti
1/2) O
3, ground 200 mesh sieves after cooling, standby.
4. a kind of high frequency ceramic filter piezoelectric ceramics as claimed in claim 1 is characterized in that: the consisting of of described piezoelectric ceramics: 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 ceramics as claimed in claim 1 is characterized in that: the consisting of of described piezoelectric ceramics: 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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|---|---|---|---|
| CN201310349033.2A CN103435344B (en) | 2013-08-13 | 2013-08-13 | Piezoceramic material for high-frequency ceramic filter |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310349033.2A CN103435344B (en) | 2013-08-13 | 2013-08-13 | Piezoceramic material for high-frequency ceramic filter |
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| Publication Number | Publication Date |
|---|---|
| CN103435344A true CN103435344A (en) | 2013-12-11 |
| CN103435344B CN103435344B (en) | 2015-04-22 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107840655A (en) * | 2017-09-25 | 2018-03-27 | 同济大学 | The preparation method of the unleaded relaxation ferroelectric ceramic of bismuth potassium titanate base of quasi- homotype phase boundary |
| 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 |
-
2013
- 2013-08-13 CN CN201310349033.2A patent/CN103435344B/en not_active Expired - Fee Related
Non-Patent Citations (3)
| Title |
|---|
| QIAN WEI ET AL.: "Morphotropic Phase Diagram and Dielectric and Ferroelectric Properties of (1-x)Ba(Sc1/2Nb1/2)O3-xPbTiO3 Solid Solution", 《CHEM. MATER》 * |
| 刁春丽等: "微波介质陶瓷的研究进展", 《中国陶瓷》 * |
| 赁敦敏等: "LiNbO3基无铅压电陶瓷的研究与进展", 《功能材料》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107840655A (en) * | 2017-09-25 | 2018-03-27 | 同济大学 | The preparation method of the unleaded relaxation ferroelectric ceramic of bismuth potassium titanate base of quasi- homotype phase boundary |
| 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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| Publication number | Publication date |
|---|---|
| CN103435344B (en) | 2015-04-22 |
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