CN102126855A - Production method of high-temperature high-power piezoelectric ceramic - Google Patents
Production method of high-temperature high-power piezoelectric ceramic Download PDFInfo
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- CN102126855A CN102126855A CN2010105506825A CN201010550682A CN102126855A CN 102126855 A CN102126855 A CN 102126855A CN 2010105506825 A CN2010105506825 A CN 2010105506825A CN 201010550682 A CN201010550682 A CN 201010550682A CN 102126855 A CN102126855 A CN 102126855A
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Abstract
The invention discloses a production method of high-temperature high-power piezoelectric ceramic by a MnO2-modified lead iridium niobate-lead zirconate-lead titanate (PYN-PZ-PT) ternary system. The production method comprises the following steps of: preparing raw materials, namely analytically pure PbO, Yb2O3, Nb2O5, ZrO2 and MnO2 and chemically pure TiO2; synthesizing clinkers by a two-step method, namely mixing Yb2O3 and Nb2O5 according to a stoichiometric ratio and performing ball milling respectively; presintering at 1,100 DEG C for 4 hours to synthesize a precursor; mixing the precursor with PbO, ZrO2, TiO2 and MnO2, and keeping the temperature at 850 DEG C for 3 hours to synthesize PYN-PZ-PT powder; performing dry pressing molding at 150MPa, sintering at 1,220 DEG C, and keeping the temperature for 3 hours; grinding and polishing a sintered sample to form a wafer with the diameter of 10 to 11mm and the thickness of 0.5mm, coating silver, and energizing at 3 to 4KV/mm in silicon oil at 120 DEG C for polarization for 30 minutes; and standing for 24 hours, and measuring the performance of the sample, namely measuring the resonant frequency, the anti-resonance frequency and the corresponding impedance, namely the absolute value of Z of the sample by a resonance-anti-resonance method, and measuring a computer electric coupling coefficient Kp, a mechanical quality factor Qm and a piezoelectric constant d33 by a quasistatic method. An optimized formula provided by the production method has higher combined mechanical and electrical properties and a higher Curie temperature, is suitable for ultrasonic transducers, and has high commercial value.
Description
Technical field
The present invention relates to be used for the piezoceramic material of ultrasonic transducer (underwater acoustic transducer, piezoelectric transformer and ultrasonic motor etc.), belong to electronic material and components and parts field.
Background technology
In general, ultrasonic transducer (underwater acoustic transducer, piezoelectric transformer and ultrasonic motor etc.) to the piezoceramic material performance demands mainly according to its drive principle and mode and fixed, for the ultrasonic transducer that is operated under the resonant condition, require piezoceramic material to satisfy following requirement: the high mechanical quality factor (Q
m) and less dielectric loss (tan δ); Require big as far as possible electromechanical coupling factor (K on this basis
p) and piezoelectric constant (d
33); Because ultrasonic transducer is worked under resonant condition, heating causes that temperature raises, and also requires piezoelectric ceramics to have high Curie temperature simultaneously, can be operated in the scope of broad to guarantee ultrasonic transducer.For this reason, require ultrasonic transducer to have good comprehensive electromechanical properties and high Curie temperature with piezoelectric ceramics.
Find that through literature search publication number is that the Chinese patent of CN1349953 discloses cadmium niobium-manganese niobium-lead zirconate-titanate (Pb (Cd to prior art
1/3Nb
2/3) O
3-Pb (Mn
1/3Nb
2/3) O
3-PbZrO
3-PbTiO
3) quaternary system high-curie temperature high-power piezoelectric ceramic, and add CeO
2Carry out modification, this ceramic systems has prepared comprehensive electromechanical properties piezoelectric ceramics preferably in conjunction with the characteristics of cadmium niobium Pb-based lanthanumdoped zirconate titanates system and manganese niobium Pb-based lanthanumdoped zirconate titanates system, and Curie temperature is up to 388 ℃.But this system deficiency is: cadmium is a kind of poisonous element, and is serious to human body harm by the air of cadmium pollution and food, do not meet requirements of green environmental protection, is difficult to use, and this system is a quaternary system, and adopts CeO
2Carry out modification, used component is more, produces waywardly, and difficulty is higher.Find also in the retrieval that publication number is that the Chinese patent of CN1061111 discloses the lead magnoniobate-manganese niobium lead acid-lead zirconates-lead titanate (Pb (Mg that is used for piezoelectric transformer
1/3Nb
2/3) O
3-Pb (Mn
1/3Nb
2/3) O
3-PbZrO
3-PbTiO
3) four-component-system piezoelectric ceramics, magnesium niobium lead zirconate titanate and niobium manganese zirconium titanium acid lead are carried out best of breed and modification, thereby obtained the quaternary system piezoelectric ceramic material of excellent performance under high-power use.But this system deficiency is: Curie temperature relatively low (350 ℃), this system also is a quaternary system, and adopts CeO
2Carry out modification with Sr, used component is more, and the production difficulty is higher.
By retrieving existing patent and document, do not find to adopt MnO
2The report of modification iridium lead niobate-lead zirconates-lead titanate three component system prescription.
Summary of the invention
The objective of the invention is at the problems referred to above: the used component of material is more, and the production difficulty is higher.Provide a kind of three component system prescription, promptly a kind of production method of high temperature high power piezoelectric ceramics with high-curie temperature and good comprehensive electromechanical properties piezoelectric ceramics.
Technical scheme of the present invention is as follows: lead zirconates-lead titanate (xPbZrO3-(1-x) PbTiO3 (x=0.52)) two component system has excellent piezoelectric property and high Curie temperature TC (～402 ℃), iridium lead niobate (Pb (Yb1/2Nb1/2) O3) is a kind of typical relaxation ferroelectric material, in relaxation ferroelectrics system, Pb (Yb
1/2Nb
1/2) O
3Has higher T
C(300 ℃), and iridium lead niobate-lead zirconates-lead titanate ((1-x-y) Pb (Yb
1/2Nb
1/2)-xPbZrO
3-yPbTiO
3(PYN-PZ-PT, x=0.42, y=0.48)) three component system has high T
C(395 ℃) and Kp value 0.61.Many studies show that:, the Mn ion is taken into account the characteristic of " soft " property and " firmly " property piezoelectric ceramics, improves Q simultaneously
m, K
pAnd d
33, Mn ion modification PZT series piezoelectric ceramic can obtain to have the high-power piezoelectric ceramic of good comprehensive electromechanical properties.
The present invention passes through MnO
2Modification iridium lead niobate-lead zirconates-lead titanate (PYN-PZ-PT) three component system is to obtain the high temperature high power piezoelectric ceramics.
This three component system is formed (molar percentage): 10% Pb (Yb
1/2Nb
1/2), 42.3% PbZrO
3, 47.7% PbTiO
3On the basis of this three component system, add the MnO of 0.4～0.6% weight percent
2
The present invention includes following steps:
1) adopts raw material: analytically pure PbO, Yb
2O
3, Nb
2O
5, ZrO
2, MnO2 and chemical pure TiO
2
2) adopt the synthetic grog of two-step approach: respectively with Yb
2O
3And Nb
2O
5By stoichiometric ratio difference mixing and ball milling; The synthetic presoma of pre-burning 4h under 1100 ℃ temperature; Again with these presomas and PbO, ZrO
2, TiO
2Mix with MnO2, be incubated the synthetic PYN-PZ-PT powder of 3h down at 850 ℃, burn till after 150MPa is dry-pressing formed, calcining system is 1220 ℃, insulation 3h;
3) sample after burning till through polishing, be polished to the disk of diameter 10～11mm, thickness 0.5mm, by silver back making alive 3～4KV/mm polarization 30min in 120 ℃ silicone oil; Place 24h.
Survey its performance after placing 24h.Resonant frequency and anti-resonance frequency and corresponding impedance with resonance-antiresonance method measure sample | Z|, computer electric coupling coefficient Kp and mechanical quality factor Q m, piezoelectric constant d
33Measure by quasi-static method.
Beneficial effect
MnO
2Modification iridium lead niobate-lead zirconates-lead titanate ternary is a kind of new piezoelectric ceramics system, can adjust its piezoelectric property in the scope of broad, and have than high-curie temperature.The optimization of C that is provided has comprehensive preferably electromechanical properties, is applicable to ultrasonic transducer, has good commercial and is worth.
Embodiment
Below by the case study on implementation detailed analysis, further specify the present invention:
Embodiment 1:
Forming (molar percentage) is: 110% Pb (Yb
1/2Nb
1/2), 42.3% PbZrO
3, 47.7% PbTiO
3On the basis of this three component system, add the MnO of 0.5% weight percent
2
Respectively with Yb
2O
3And Nb
2O
5By stoichiometric ratio difference mixing and ball milling, the synthetic presoma of pre-burning 4h under 1100 ℃ temperature.Again with these presomas and PbO, ZrO
2, TiO
2Mix with MnO2, be incubated the synthetic PYN-PZ-PT powder of 3h down at 850 ℃, burn till after 150MPa is dry-pressing formed, calcining system is 1220 ℃, insulation 3h.
Electromechanical properties are: Kp=0.58, Qm=1215, d
33=356pC/N, tan δ=0.0035, Tc=378 ℃.This prescription Kp and d
33Higher, the Qm value is higher than 1000, has good comprehensive electromechanical properties, is screening formulation.
Embodiment 2:
Forming (molar percentage) is: 110% Pb (Yb
1/2Nb
1/2), 42.3% PbZrO
3, 47.7% PbTiO
3On the basis of this three component system, add the MnO of 0.5% weight percent
2
Respectively with Yb
2O
3And Nb
2O
5By stoichiometric ratio difference mixing and ball milling, the synthetic presoma of pre-burning 4h under 1100 ℃ temperature.Again with these presomas and PbO, ZrO
2, TiO
2Mix with MnO2, be incubated the synthetic PYN-PZ-PT powder of 3h down at 850 ℃, burn till after 150MPa is dry-pressing formed, calcining system is 1220 ℃, insulation 3h.
Electromechanical properties are: electromechanical properties are: Kp=0.54, Qm=850, d
33=312pC/N, tan δ=0.0052, Tc=383 ℃.
Embodiment 3:
Forming (molar percentage) is: 110% Pb (Yb
1/2Nb
1/2), 42.3% PbZrO
3, 47.7% PbTiO
3On the basis of this three component system, add the MnO of 0.6% weight percent
2
Respectively with Yb
2O
3And Nb
2O
5By stoichiometric ratio difference mixing and ball milling, the synthetic presoma of pre-burning 4h under 1100 ℃ temperature.Again with these presomas and PbO, ZrO
2, TiO
2Mix with MnO2, be incubated the synthetic PYN-PZ-PT powder of 3h down at 850 ℃, burn till after 150MPa is dry-pressing formed, calcining system is 1220 ℃, insulation 3h.
Electromechanical properties are: Kp=0.56, Qm=1005, d
33=332pC/N, tan δ=0.0042, Tc=371 ℃.
Above embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to the above embodiments.
Claims (2)
1. the production method of a high temperature high power piezoelectric ceramics is characterized in that: pass through MnO
2Modification iridium lead niobate-lead zirconates-lead titanate (PYN-PZ-PT) three component system: may further comprise the steps:
1) adopts raw material: analytically pure PbO, Yb
2O
3, Nb
2O
5, ZrO
2, MnO2 and chemical pure TiO
2
2) adopt the synthetic grog of two-step approach: respectively with Yb
2O
3And Nb
2O
5By stoichiometric ratio difference mixing and ball milling; The synthetic presoma of pre-burning 4h under 1100 ℃ temperature; Again with these presomas and PbO, ZrO
2, TiO
2Mix with MnO2, be incubated the synthetic PYN-PZ-PT powder of 3h down at 850 ℃, burn till after 150MPa is dry-pressing formed, calcining system is 1220 ℃, insulation 3h;
3) sample after burning till through polishing, be polished to the disk of diameter 10～11mm, thickness 0.5mm, by silver back making alive 3～4KV/mm polarization 30min in 120 ℃ silicone oil; Place 24h.
2. production method according to claim 1, it is characterized in that: described step 3) is surveyed its performance after placing 24h, survey resonant frequency and the anti-resonance frequency and the corresponding impedance of its performance employing resonance-antiresonance method measure sample | Z|, computer electric coupling coefficient Kp and mechanical quality factor Q m, piezoelectric constant d
33Measure by quasi-static method.
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|---|---|---|---|
| CN2010105506825A CN102126855A (en) | 2010-11-19 | 2010-11-19 | Production method of high-temperature high-power piezoelectric ceramic |
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|---|---|---|---|
| CN2010105506825A CN102126855A (en) | 2010-11-19 | 2010-11-19 | Production method of high-temperature high-power piezoelectric ceramic |
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| CN102126855A true CN102126855A (en) | 2011-07-20 |
Family
ID=44265178
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104823354A (en) * | 2013-02-14 | 2015-08-05 | 株式会社村田制作所 | Parameter derivation method |
| CN111848164A (en) * | 2020-06-22 | 2020-10-30 | 华南理工大学 | Piezoelectric ceramic with high transverse resonant frequency and temperature stability as well as preparation method and application thereof |
| CN112142466A (en) * | 2019-06-26 | 2020-12-29 | 中国科学院上海硅酸盐研究所 | Lead niobate ytterbium acid based antiferroelectric ceramic material and preparation method thereof |
Citations (4)
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|---|---|---|---|---|
| US20070252484A1 (en) * | 2004-12-22 | 2007-11-01 | Murata Manufacturing Co., Ltd. | Piezoelectric ceramic composition and piezoelectric actuator |
| CN101098836A (en) * | 2005-01-14 | 2008-01-02 | 株式会社村田制作所 | Piezoelectric ceramic composition and piezoelectric actuator |
| CN101456732A (en) * | 2008-12-31 | 2009-06-17 | 中国科学院上海硅酸盐研究所 | High temperature and high sensitivity piezoelectric ceramic material and preparation method thereof |
| CN101798219A (en) * | 2010-02-26 | 2010-08-11 | 上海海事大学 | Piezoelectric ceramics for underwater acoustic transducer and preparation method thereof |
-
2010
- 2010-11-19 CN CN2010105506825A patent/CN102126855A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070252484A1 (en) * | 2004-12-22 | 2007-11-01 | Murata Manufacturing Co., Ltd. | Piezoelectric ceramic composition and piezoelectric actuator |
| CN101098836A (en) * | 2005-01-14 | 2008-01-02 | 株式会社村田制作所 | Piezoelectric ceramic composition and piezoelectric actuator |
| CN101456732A (en) * | 2008-12-31 | 2009-06-17 | 中国科学院上海硅酸盐研究所 | High temperature and high sensitivity piezoelectric ceramic material and preparation method thereof |
| CN101798219A (en) * | 2010-02-26 | 2010-08-11 | 上海海事大学 | Piezoelectric ceramics for underwater acoustic transducer and preparation method thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104823354A (en) * | 2013-02-14 | 2015-08-05 | 株式会社村田制作所 | Parameter derivation method |
| CN112142466A (en) * | 2019-06-26 | 2020-12-29 | 中国科学院上海硅酸盐研究所 | Lead niobate ytterbium acid based antiferroelectric ceramic material and preparation method thereof |
| CN112142466B (en) * | 2019-06-26 | 2021-05-25 | 中国科学院上海硅酸盐研究所 | Lead niobate ytterbium acid based antiferroelectric ceramic material and preparation method thereof |
| CN111848164A (en) * | 2020-06-22 | 2020-10-30 | 华南理工大学 | Piezoelectric ceramic with high transverse resonant frequency and temperature stability as well as preparation method and application thereof |
| CN111848164B (en) * | 2020-06-22 | 2021-10-26 | 华南理工大学 | Piezoelectric ceramic with high transverse resonant frequency and temperature stability as well as preparation method and application thereof |
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Application publication date: 20110720 |