CN103524129A - Piezoceramic material for ultrasonic emission-type transducers and preparation method - Google Patents
Piezoceramic material for ultrasonic emission-type transducers and preparation method Download PDFInfo
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- CN103524129A CN103524129A CN201310462475.8A CN201310462475A CN103524129A CN 103524129 A CN103524129 A CN 103524129A CN 201310462475 A CN201310462475 A CN 201310462475A CN 103524129 A CN103524129 A CN 103524129A
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Abstract
The invention relates to the technical field of inorganic non-metallic materials, and especially relates to a piezoceramic material for ultrasonic emission-type transducers and a preparation method. The piezoceramic material is characterized in that the formula of the piezoceramic material comprises xBiFeO3-y(Pb0.90Ba0.05Sr0.05)(Zr0.54Ti0.46)O3, 0.01-0.6wt.% of Cr2O3, 0.01-0.7wt.% of MnO2, 0.01-0.9wt.% of Fe2O3, 0.01-6wt.% of (0.15B2O3-0.125Bi2O3-0.45CdO) glass powder, wherein, x is more than or equal to 0.005 and less than or equal to 0.2mol, x+y=1; wherein, BiFeO3, (Pb0.90Ba0.05Sr0.05)(Zr0.54Ti0.46)O3 and BBC glass powder are synthesized through a solid phase method with conventional chemical raw materials respectively. The piezoceramic material with high stabilization and high voltage performances is prepared and obtained through a conventional solid phase method preparation method for piezoceramic material by utilization of common chemical raw materials. The piezoceramic material is suitable for preparation of ultrasonic emission-type transducers.
Description
Technical field
The present invention relates to technical field of inorganic nonmetallic materials, refer in particular to piezoceramic material and preparation method thereof for a kind of ultrasound emission type transverter, it adopts the preparation method of conventional solid phase method piezoelectric ceramics, utilize general chemistry raw material, prepare high stable high tension performance piezoelectric ceramics, this piezoelectric ceramics is suitable for preparing ultrasound emission type transverter.
Background technology
Piezoelectric ceramics has good piezoelectric effect, in function ceramics, to apply a class very widely, 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, making the devices such as ultrasonic transducer is mainly Pb-based lanthanumdoped zirconate titanates base piezoelectric ceramic, some piezoelectric properties are good, but its time less stable, prolongation due to the time, easily produce the larger drift of resonant frequency, the larger variation of relative bandwidth, be difficult to meet the requirement of high tension performance and high time stability, some piezoelectric properties are not so good, and some specific inductivity are lower, and some dielectric losses are larger, and some Qms are lower, can not meet the requirement of the devices such as ultrasound emission type transverter, in order to improve the performance of piezoceramic material, often adopt two kinds of approach: the one, by adding ternary or quaternary to reach the object of modification to form novel material in body material, the 2nd, different on the impact of material property according to different dopant ions, material is carried out to doping vario-property, the present invention obtains the bismuth ferrite Pb-based lanthanumdoped zirconate titanates ternary system piezoelectric ceramics of high time stable high voltage electrical property, can be for the preparation of devices such as ultrasound emission type transverters, 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 1000 ~ 1030 ℃ of left and right, 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 type transverter piezoelectric ceramics, its formula is: xBiFeO
3-y (Pb
0.90ba
0.05sr
0.05) (Zr
0.54ti
0.46) O
3+ 0.01 ~ 0.6wt.%Cr
2o
3+ 0.01 ~ 0.7wt.%MnO
2+ 0.01 ~
0.9wt.%Fe
2o
3+ 0.01 ~ 6wt.% (0.15B
2o
3-0.125Bi
2o
3-0.45CdO) glass powder (is called for short: BBC glass powder); Wherein, 0.005≤x≤0.2 mol, x+y=1; BiFeO wherein
3, (Pb
0.90ba
0.05sr
0.05) (Zr
0.54ti
0.46) O
3(0.15B
2o
3-0.125Bi
2o
3-0.45CdO) glass powder is respectively to adopt conventional chemical feedstocks synthetic with solid phase method.
Cr
2o
3, MnO
2, Fe
2o
3be respectively xBiFeO with the addition of BBC glass powder
3-y (Pb
0.90ba
0.05sr
0.05) (Zr
0.54ti
0.46) O
30.01 ~ 0.6%, 0.01 ~ 0.7%, 0.01 ~ 0.9% and 0.01 ~ 6% of quality.
The specific inductivity of described piezoelectric ceramics is 1293-1312, Qm (Q
m) be 1020-1086, electromechanical coupling factor (K radially
p) be 0.64-0.67, piezoelectric strain constant (d
33) be 308-325pC/N, resonant frequency time stability is good, its velocity of variation (t after aging 200 hours
fr) be 0.002%-0.004%, dielectric loss (tan δ) is 0.032%-0.043%.
(the Pb that piezoelectric ceramics of the present invention is used
0.90ba
0.05sr
0.05) (Zr
0.54ti
0.46) O
3preparation process comprise: by conventional chemical feedstocks Pb
3o
4, BaCO
3, SrCO
3, ZrO
2and TiO
2according to: the molar ratio ingredient of 0.9/3:0.05:0.05:0.54:0.46, after ground and mixed is even, put into alumina crucible in 850 ~ 900 ℃ of insulations 120 minutes, solid state reaction is synthesized (Pb
0.90ba
0.05sr
0.05) (Zr
0.54ti
0.46) O
3, ground 200 mesh sieves after cooling, standby.
The BiFeO that piezoelectric ceramics of the present invention is used
3preparation process comprise: by conventional chemical feedstocks Bi
2o
3and Fe
2o
3according to: the molar ratio ingredient of 1/2:1/2, after ground and mixed is even, put into alumina crucible in 500 ~ 550 ℃ of insulations 120 minutes, solid state reaction is synthesized BiFeO
3, ground 200 mesh sieves after cooling, standby.
(the 0.15B that piezoelectric ceramics of the present invention is used
2o
3-0.125Bi
2o
3-0.45CdO) (be called for short: BBC) preparation process of glass powder comprises: by conventional chemical feedstocks B
2o
3, Bi
2o
3according to 0.15:0.125:0.45 molar ratio ingredient, ground and mixed is put into alumina crucible after evenly and is incubated 120 minutes in 600 ℃ ~ 650 ℃ with CdO, quenching in water then, and solid state reaction is synthesized BBC glass powder, grinds 200 mesh sieves after cooling, standby.
The present invention adopts conventional solid phase method pottery preparation technology, first by formula, prepares burden admixtion ball milling powder
Broken mixing, after drying, adds tackiness agent granulation, then is pressed into green sheet, then in air, carry out binder removal and sintering, after insulation naturally cooling, obtain bismuth ferrite Pb-based lanthanumdoped zirconate titanates ternary system piezoelectric ceramics, on pottery by electrode, then polarization, aging, surveys performance.
In above-mentioned water, ultrasound emission type transverter preferably adopts following two kinds of schemes with the formula of piezoelectric ceramics:
xBiFeO
3-y(Pb
0.90Ba
0.05Sr
0.05)(Zr
0.54Ti
0.46)O
3+0.05~0.5wt.%Cr
2O
3+0.10~0.6wt.%
MnO
2+ 0.08 ~ 0.7wt.%Fe
2o
3+ 0.08 ~ 5wt.% BBC glass powder; Wherein, 0.008≤x≤0.15 mol, x+y=1.
xBiFeO
3-y(Pb
0.90Ba
0.05Sr
0.05)(Zr
0.54Ti
0.46)O
3+0.08~0.4wt.%Cr
2O
3+0.10~0.5wt.%
MnO
2+ 0.08 ~ 0.6wt.%Fe
2o
3+ 0.10 ~ 4wt.% BBC glass powder; Wherein, 0.010≤x≤0.10 mol, x+y=1.
Compared with prior art, tool has the following advantages in the present invention:
1, the specific inductivity of prepared piezoelectric ceramics is about 1300 left and right, Qm (Q
m) be greater than 1000, electromechanical coupling factor (K radially
p) be 0.65 left and right, piezoelectric strain constant (d
33) being greater than 300pC/N, 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 0.05%; 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 ultrasound emission type transverter.
3, this pottery adopts conventional solid phase method piezoelectric ceramics preparation technology to be prepared, and the raw material using is conventional chemical feedstocks, and cost of manufacture is low; The sintering temperature of piezoelectric ceramics of the present invention is 1000 ~ 1030 ℃, 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.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, and pre-synthesis BiFeO
3, (Pb
0.90ba
0.05sr
0.05) (Zr
0.54ti
0.46) O
3with BBC glass powder, by above-mentioned formula batching, mixing, with distilled water or deionized water, adopt planetary ball mill ball milling to mix in the material preparing, material: ball: water=1:3:(0.6 ~ 1.0), after ball milling 4 ~ 8 hours, dry to obtain dry mash, in dry mash, adding the concentration that accounts for its weight 5 ~ 8% is the polyvinyl alcohol solution of 10% (weight percent), carry out granulation, mixed rear mistake 40 mesh sieves, under 20 ~ 30Mpa pressure, carrying out dry-pressing again and become green sheet, is then at 750 ~ 850 ℃, to be incubated 1 ~ 4 hour to carry out binder removal in temperature, and temperature rise rate is 50 ~ 100 ℃/h; Then sample is placed in to alumina crucible, airtight sintering, sintering temperature is 1000 ~ 1030 ℃, soaking time is 1 ~ 2 hour, obtains ceramic plate; Ceramic plate is two sides coating silver electrode after grinding and polishing, and about 135 ℃ polarization in silicone oil, and polarized electric field is 3000 ~ 5000 volts/mm, and the polarization time is 15 ~ 20 minutes; Polarize complete, test resonant frequency, through 200 hours test resonant frequencies of overaging, calculates 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 the specific inductivity of prepared piezoelectric ceramics (ε) is about 1300 left and right as can be seen from Table 2, Qm (Q
m) be greater than 1000, electromechanical coupling factor (K radially
p) be 0.65 left and right, piezoelectric strain constant (d
33) being greater than 300pC/N, 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 0.05%.
Table 1 embodiments of the invention are the formula 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 (8)
1. a ultrasound emission type transverter piezoelectric ceramics, is characterized in that the formula of described piezoelectric ceramics is: xBiFeO
3-y (Pb
0.90ba
0.05sr
0.05) (Zr
0.54ti
0.46) O
3+ 0.01 ~ 0.6wt.%Cr
2o
3+ 0.01 ~ 0.7wt.%MnO
2+ 0.01 ~ 0.9wt.%Fe
2o
3+ 0.01 ~ 6wt.% (0.15B
2o
3-0.125Bi
2o
3-0.45CdO) glass powder; Wherein, 0.005≤x≤0.2 mol, x+y=1; BiFeO wherein
3, (Pb
0.90ba
0.05sr
0.05) (Zr
0.54ti
0.46) O
3(0.15B
2o
3-0.125Bi
2o
3-0.45CdO) glass powder is respectively to adopt conventional chemical feedstocks synthetic with solid phase method; Cr
2o
3, MnO
2, Fe
2o
3be respectively xBiFeO with the addition of BBC glass powder
3-y (Pb
0.90ba
0.05sr
0.05) (Zr
0.54ti
0.46) O
30.01 ~ 0.6%, 0.01 ~ 0.7%, 0.01 ~ 0.9% and 0.01 ~ 6% of quality.
2. a kind of ultrasound emission type transverter piezoelectric ceramics as claimed in claim 1, is characterized in that: the specific inductivity of described piezoelectric ceramics is 1293-1312, Qm (Q
m) be 1020-1086, electromechanical coupling factor (K radially
p) be 0.64-0.67, piezoelectric strain constant (d
33) be 308-325pC/N, resonant frequency time stability is good, its velocity of variation (t after aging 200 hours
fr) be 0.002%-0.004%, dielectric loss (tan δ) is 0.032%-0.043%.
3. a kind of ultrasound emission type transverter piezoelectric ceramics as claimed in claim 1, is characterized in that: described (Pb
0.90ba
0.05sr
0.05) (Zr
0.54ti
0.46) O
3preparation process as follows: by conventional chemical feedstocks Pb
3o
4, BaCO
3, SrCO
3, ZrO
2and TiO
2according to: the molar ratio ingredient of 0.9/3:0.05:0.05:0.54:0.46, after ground and mixed is even, put into alumina crucible in 850 ~ 900 ℃ of insulations 120 minutes, solid state reaction is synthesized (Pb
0.90ba
0.05sr
0.05) (Zr
0.54ti
0.46) O
3, ground 200 mesh sieves after cooling, standby.
4. a kind of ultrasound emission type transverter piezoelectric ceramics as claimed in claim 1, is characterized in that: described BiFeO
3preparation process as follows: by conventional chemical feedstocks Bi
2o
3and Fe
2o
3according to: the molar ratio ingredient of 1/2:1/2, after ground and mixed is even, put into alumina crucible in 500 ~ 550 ℃ of insulations 120 minutes, solid state reaction is synthesized BiFeO
3, ground 200 mesh sieves after cooling, standby.
5. a kind of ultrasound emission type transverter piezoelectric ceramics as claimed in claim 1, is characterized in that: described (0.15B
2o
3-0.125Bi
2o
3-0.45CdO) preparation process of glass powder is as follows: by conventional chemical feedstocks B
2o
3, Bi
2o
3according to 0.15:0.125:0.45 molar ratio ingredient, ground and mixed is put into alumina crucible after evenly and is incubated 120 minutes in 600 ℃ ~ 650 ℃ with CdO, quenching in water then, and solid state reaction is synthesized BBC glass powder, grinds 200 mesh sieves after cooling, standby.
6. a kind of ultrasound emission type transverter piezoelectric ceramics as claimed in claim 1, is characterized in that the formula of described piezoelectric ceramics is: xBiFeO
3-y (Pb
0.90ba
0.05sr
0.05) (Zr
0.54ti
0.46) O
3+ 0.05 ~ 0.5wt%Cr
2o
3+ 0.10 ~ 0.6wt%MnO
2
+ 0.08 ~ 0.7wt%Fe
2o
3+ 0.08 ~ 5wt% BBC glass powder; Wherein, 0.008≤x≤0.15 mol, x+y=1.
7. a kind of ultrasound emission type transverter piezoelectric ceramics as claimed in claim 1, is characterized in that the formula of described piezoelectric ceramics is: xBiFeO
3-y (Pb
0.90ba
0.05sr
0.05) (Zr
0.54ti
0.46) O
3+ 0.08 ~ 0.4wt%Cr
2o
3+ 0.10 ~ 0.5wt%MnO
2
+ 0.08 ~ 0.6wt%Fe
2o
3+ 0.10 ~ 4wt%BBC glass powder; Wherein, 0.010≤x≤0.10 mol, x+y=1.
8. the preparation method of piezoelectric ceramics for a kind of ultrasound emission type transverter as claimed in claim 1, is characterized in that comprising the steps: to adopt conventional chemical feedstocks, and pre-synthesis BiFeO
3, (Pb
0.90ba
0.05sr
0.05) (Zr
0.54ti
0.46) O
3with BBC glass powder, by formula batching, mixing, with distilled water or deionized water, adopt planetary ball mill ball milling to mix in the material preparing, material: ball: water=1:3:(0.6 ~ 1.0), after ball milling 4 ~ 8 hours, dry to obtain dry mash, in dry mash, add and account for the polyvinyl alcohol solution that the concentration of its weight 5 ~ 8% is 10wt%, carry out granulation, mixed rear mistake 40 mesh sieves, under 20 ~ 30Mpa pressure, carrying out dry-pressing again and become green sheet, is then at 750 ~ 850 ℃, to be incubated 1 ~ 4 hour to carry out binder removal in temperature, and temperature rise rate is 50 ~ 100 ℃/h; Then sample is placed in to alumina crucible, airtight sintering, sintering temperature is 1000 ~ 1030 ℃, soaking time is 1 ~ 2 hour, obtains ceramic plate.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105503164A (en) * | 2014-10-16 | 2016-04-20 | 桂林电子科技大学 | High insulation bismuth ferrite based high temperature piezoelectric glass ceramic composite material and preparation method thereof |
| CN110511023A (en) * | 2019-09-30 | 2019-11-29 | 海鹰企业集团有限责任公司 | A kind of novel high-stability piezoelectric material and preparation method thereof |
| CN116283281A (en) * | 2023-04-07 | 2023-06-23 | 中国科学院上海硅酸盐研究所 | Piezoelectric driver material with bidirectional strain and preparation method thereof |
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| US20060066180A1 (en) * | 2004-09-29 | 2006-03-30 | Ngk Insulators, Ltd. | Piezoelectric/electrostrictive porcelain composition, piezoelectric/electrostrictive article, and piezoelectric/electrostrictive film type element |
| KR20070088274A (en) * | 2005-04-28 | 2007-08-29 | 가부시키가이샤 무라타 세이사쿠쇼 | Piezoelectric ceramic composition and piezoelectric ceramic electronic component |
| CN101255053A (en) * | 2008-04-08 | 2008-09-03 | 同济大学 | High-temperature single-phase ferromagnetic-ferroelectric multiferroics ceramic material and preparation method thereof |
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2013
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| US20060066180A1 (en) * | 2004-09-29 | 2006-03-30 | Ngk Insulators, Ltd. | Piezoelectric/electrostrictive porcelain composition, piezoelectric/electrostrictive article, and piezoelectric/electrostrictive film type element |
| KR20070088274A (en) * | 2005-04-28 | 2007-08-29 | 가부시키가이샤 무라타 세이사쿠쇼 | Piezoelectric ceramic composition and piezoelectric ceramic electronic component |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105503164A (en) * | 2014-10-16 | 2016-04-20 | 桂林电子科技大学 | High insulation bismuth ferrite based high temperature piezoelectric glass ceramic composite material and preparation method thereof |
| CN110511023A (en) * | 2019-09-30 | 2019-11-29 | 海鹰企业集团有限责任公司 | A kind of novel high-stability piezoelectric material and preparation method thereof |
| CN116283281A (en) * | 2023-04-07 | 2023-06-23 | 中国科学院上海硅酸盐研究所 | Piezoelectric driver material with bidirectional strain and preparation method thereof |
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