CN103011815A - Ternary ferroelectric solid solution lead lutecium niobate-lead magnesium niobate-lead titanate - Google Patents
Ternary ferroelectric solid solution lead lutecium niobate-lead magnesium niobate-lead titanate Download PDFInfo
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- CN103011815A CN103011815A CN201210519826XA CN201210519826A CN103011815A CN 103011815 A CN103011815 A CN 103011815A CN 201210519826X A CN201210519826X A CN 201210519826XA CN 201210519826 A CN201210519826 A CN 201210519826A CN 103011815 A CN103011815 A CN 103011815A
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Abstract
The invention relates to a ferroelectric solid solution lead lutecium niobate-lead magnesium niobate-lead titanate and a preparation method and application thereof. Such a solid solution system is determined to be a perovskite structure through X-ray powder diffraction, and ferroelectricity, dielectricity and piezo-electricity of the solid solution system are analyzed by using ferroelectric, dielectric and piezoelectric measurement. Based on measurement and analysis of the structure and dielectricity of the solid solution system, MPB composition of the ternary ferroelectric solid solution system is obtained. The system has good piezoelectric and electromechanical properties, a high Curie temperature, good thermal stability and wide application prospects.
Description
Technical field
The present invention relates to a kind of novel ferroelectric/piezoceramic material.Particularly, the present invention relates to and have MPB structure and the relatively high ferroelectric material xPb (Lu of Curie temperature
1/2Nb
1/2) O
3-yPb (Mg
1/3Nb
2/3) O
3-(1-x-y) PbTiO
3, note by abridging and be PLN-PMN-PT or PLMNT, and preparation method, structure and the electric property of pottery; Belong to functional materials and learn the field.
Background technology
Ferroelectric/piezoceramic material is a kind of polycrystal with piezoelectric property, is the important component part of informational function pottery.It has electromechanical coupling factor height, low price, is easy to the advantages such as batch production, be widely used in the every field of social production, especially in ultrasonic field and electronic science and technology field, piezoceramic material is in absolute advantage ascendancy gradually.PZT(Pb (Zr
1-xTi
x) O
3) pottery is a kind of conventional piezoelectric materials that is widely used in the aspects such as ultrasonic Transducers in Medicine, underwater acoustic transducer, driving mechanism and ultrasonic motor.Since the 1950's, played an important role in the piezoelectricity Application Areas.Mainly be because there is accurate homotype phase boundary (MPB) in the PZT pottery, and high, the advantages such as piezoelectricity is strong, good stability of MPB zone Curie temperature, more important is to be easy to by doping vario-property to satisfy different needs.
Along with going deep into of MPB research, new MPB is found in the Relaxor-PT material.Relaxation ferroelectric can form sosoloid and show the dielectric and piezoelectric properties better than PZT, wherein more typically is exactly (1-x) Pb (Mg
1/3Nb
2/3)-xPbTiO
3(PMNT) and (1-x) Pb (Zn
1/3Nb
2/3)-xPbTiO
3(PZNT) system.Such monocrystal material component shows high electromechanical coupling factor (k near MPB
3390%), extra-high voltage coefficient (d
332000pC/N) and large strain (〉 1%) and become the core piezoelectric of ultrasonic transducer, sensor and driving mechanism of a new generation.Although PMNT and PZNT have these excellent character, the Curie temperature that it is relatively low and lower tripartite Tetragonal temperature make the easy umpolarization of these materials, and then have reduced its piezoelectricity use temperature scope.In order to overcome this defective, mainly ternary and the multicomponent system that contains PMN or PZN is studied PYN-PMN-PT, PSN-PMN-PZT, PSN-PZN-PZT, PNN-PZN-PT, PZN-PZT etc. in the world in recent years.
The PLN pottery is typical antiferroelectric, at 270 ° of C paraelectric phase-antiferroelectric phase transformation occurs, and can form accurate homotype phase boundary region with PT.Pb (Lu
1/2Nb
1/2) O
3-xPbTiO
3(PLNT) be to have at present a relatively high relaxation ferroelectric of Curie temperature, the researchs about PLNT monocrystalline and pottery have been done in a large number by our seminar before, and the PLNT monocrystalline has shown the Curie temperature of superelevation and piezoelectric property (E preferably
c~ 360 ℃, d
33~ 1630pc/N, k
33~ 0.8), PLNT will show huge prospect and value in the piezoelectricity application facet of high-temperature field.
Based on this, we want to study PLN-PMN-PT ternary ferroelectric system by introducing PLN, carry out the structure of PLN-PMN-PT ternary system different components and the systematic study of dielectric and piezoelectric properties, in the hope of obtaining the novel ferroelectric/piezoelectric of excellent combination property.
Summary of the invention
The object of the invention is to explore a kind of brand-new ferroelectric sosoloid is xPb (Lu
1/2Nb
1/2) O
3-yPb (Mg
1/3Nb
2/3) O
3-(1-x-y) PbTiO
3, be called for short PLN-PMN-PT or PLMNT.
For realizing the object of the invention, the present invention adopts following technical scheme:
The present invention is a kind of ferroelectric sosoloid niobium lutetium lead plumbate-PMN-PT, it is characterized in that: this sosoloid chemical formula is xPb (Lu
1/2Nb
1/2) O
3-yPb (Mg
1/3Nb
2/3) O
3-(1-x-y) PbTiO
3(0＜x＜1,0＜y＜1) belongs to typical perovskite structure.There is accurate homotype phase boundary (MPB) district in this solid solution ceramic, and its compositing range is y=0.30,0.26＜x＜0.30; Y=0.20,0.35＜x＜0.39.
The present invention adopts the preparation of secondary synthesis method, comprises the steps: at first with magnesium oxide (MgO) and niobium oxides (Nb
2O
5) by stoichiometric ratio weighing (wherein MgO excessive 2%), obtain MgNb at 1150 ℃ of calcining 2h
2O
6Powder; With lutecium oxide (Lu
2O
3) and niobium oxides by stoichiometric ratio weighing (Lu wherein
2O
3Excessive 1%) obtains LuNbO at 1150 ℃ of calcining 2h
4Presoma; Then with MgNb
2O
6, LuNbO
4, PbO and TiO
2After (wherein PbO excessive 2%) mixed, 850 ° of C calcined 4h, obtain the PLMNT pre-synthesis powder of perovskite structure; With pre-synthesis powder ball milling, oven dry, add the PVA of 5wt%, 300-500 ℃ binder removal 1-3 hour; 1050 ° of C-1100 ° of C sintering 3 hours, obtain the PLMNT ceramics sample.
The purposes of the ferroelectric sosoloid niobium lutetium lead plumbate-PMN-PT of the present invention's preparation is characterized in that: this material is used for the especially device in piezoelectricity field of function material component field.
The present invention is based on and explores novel high temperature, the high power range of being applicable to, and the ferroelectric sosoloid system of piezoelectric property excellence carries out.PLMNT ternary ceramics with the preparation of secondary synthesis method has pure perovskite structure, extraordinary thermostability.By the structure of PLMNT ternary system and the systematic study of electric property, there is the MPB structure with change of component in the PLMNT system, under the PMN (20%, 30%) of certain content, PLN content is tripartite perovskite structure when more, PLN content is transitioned into cubic perovskite structure when less, by the analysis of XRD powdery diffractometry and dielectric temperature spectrum, the MPB structure of the ternary system of depicting be a broadening to three parts mutually crooked three parts, the zone of Tetragonal coexistence.When being 30%PMN for component, near the MPB district, the Curie temperature T of PLMNT ternary system
c~ 265-290 ℃, three parts-Tetragonal temperature T
RtBetween ~ 155-75 ℃, coercive field E
c~ 12-24 kV/cm, piezoelectric coefficient d
33~ 240-460 pC/N; The PLMNT ternary ceramics has shown relaxation behavior, and specific inductivity is with frequency dispersion, moves to the high temperature direction with the increase Curie temperature of frequency.
Embodiment
Example 1: adopt the preparation of secondary synthesis method, concrete steps:
A) magnesium oxide (MgO) and niobium oxides (Nb
2O
5) by stoichiometric ratio weighing (wherein MgO excessive 2%), obtain MgNb at 1150 ℃ of calcining 2h
2O
6Powder;
B) lutecium oxide (Lu
2O
3) and niobium oxides by stoichiometric ratio weighing (Lu wherein
2O
3Excessive 1%) obtains LuNbO at 1150 ℃ of calcining 2h
4Presoma;
C) MgNb
2O
6, LuNbO
4, PbO and TiO
2After (wherein PbO excessive 2%) mixed, 850 ° of C calcined 4h, obtain the xPb (Lu of perovskite structure
1/2Nb
1/2) O3-yPb (Mg
1/3Nb
2/3) O
3-(1-x-y) PbTiO
3The pre-synthesis powder;
D) with pre-synthesis powder ball milling, oven dry, add the PVA of 5wt%, 300-500 ℃ binder removal 1-3 hour;
E) 1050 ° of C-1100 ° of C sintering 3 hours, obtain xPb (Lu
1/2Nb
1/2) O3-yPb (Mg
1/3Nb
2/3) O
3-(1-x-y) PbTiO
3Ceramics sample.
The sample that more than obtains is the ternary ferroelectric pottery of the present invention's development.
Example 2: the structure of pottery is determined.
Adopt X-ray powder diffraction, determine the structure of pottery.Instrument is Japanese RIGAKU-DMAX2500 powder diffractometer (Cu target, λ=0.154056 nm, graphite monochromator), and concrete test condition is under the room temperature, and the scope of taking measurement of an angle is 10-80
o, the step-length of employing is 0.02
o(2 θ), per minute 7
o
Example 3: the electricity performance measurement of pottery.
With ceramics sample wear down, polishing, the silver slurry is coated on the two sides, is used for the measurement of ferroelectricity and dielectricity.
The measurement of dielectricity: instrument is alpha's dielectric/impedance Analytical high resolution instrument (Novolcontrol, GmbH), temperature-measuring range-150 ~ 500
oC, range of frequency 0.01 ~ 100 kHz, small-signal test voltage 1Vrms.
Ferroelectric measurement: instrument is the ferroelectric measuring systems of TF 2000 standards, and temperature condition is room temperature, and it is 2 Hz that institute adds frequency.
Claims (4)
1. ternary ferroelectric sosoloid niobium lutetium lead plumbate-PMN-PT, it is characterized in that: this sosoloid chemical formula is xPb (Lu
1/2Nb
1/2) O3-yPb (Mg
1/3Nb
2/3) O
3-(1-x-y) PbTiO
3(0＜x＜1,0＜y＜1) belongs to typical perovskite structure.
2. ferroelectric sosoloid niobium lutetium lead plumbate-PMN-PT as claimed in claim 1 is characterized in that: there is accurate homotype phase boundary (MPB) district in this solid solution ceramic, and its compositing range is y=0.30,0.26＜x＜0.30; Y=0.20,0.35＜x＜0.39.
3. the preparation method of a ferroelectric sosoloid niobium lutetium lead plumbate-PMN-PT claimed in claim 1 adopts the preparation of secondary synthesis method, comprises the steps:
A) magnesium oxide (MgO) and niobium oxides (Nb
2O
5) by stoichiometric ratio weighing (wherein MgO excessive 2%), obtain MgNb at 1150 ℃ of calcining 2h
2O
6Powder;
B) lutecium oxide (Lu
2O
3) and niobium oxides by stoichiometric ratio weighing (Lu wherein
2O
3Excessive 1%) obtains LuNbO at 1150 ℃ of calcining 2h
4Presoma;
C) MgNb
2O
6, LuNbO
4, PbO and TiO
2After (wherein PbO excessive 2%) mixed, 850 ° of C calcined 4h, obtain the xPb (Lu of perovskite structure
1/2Nb
1/2) O3-yPb (Mg
1/3Nb
2/3) O
3-(1-x-y) PbTiO
3The pre-synthesis powder;
D) with pre-synthesis powder ball milling, oven dry, add the PVA of 5wt%, 300-500 ℃ binder removal 1-3 hour;
E) 1050 ° of C-1100 ° of C sintering 3 hours, obtain xPb (Lu
1/2Nb
1/2) O3-yPb (Mg
1/3Nb
2/3) O
3-(1-x-y) PbTiO
3Ceramics sample.
4. the purposes of a ferroelectric sosoloid niobium lutetium lead plumbate-PMN-PT claimed in claim 1 is characterized in that: this material is used for the especially device in piezoelectricity field of function material component field.
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|---|---|---|---|
| CN201210519826.XA CN103011815B (en) | 2012-12-06 | 2012-12-06 | Ternary ferroelectric sosoloid niobium lutetium lead plumbate lead magnesio-niobate lead titanates |
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|---|---|---|---|
| CN201210519826.XA CN103011815B (en) | 2012-12-06 | 2012-12-06 | Ternary ferroelectric sosoloid niobium lutetium lead plumbate lead magnesio-niobate lead titanates |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103641478A (en) * | 2013-11-28 | 2014-03-19 | 中国科学院福建物质结构研究所 | Ferroelectric piezoelectric ceramic material of large-power energy transducer and preparation method thereof |
| CN104372409A (en) * | 2013-08-14 | 2015-02-25 | 中国科学院上海硅酸盐研究所 | Ternary relaxor-based ferroelectric piezoelectric single crystal and growing method thereof |
| CN109650888A (en) * | 2018-12-27 | 2019-04-19 | 哈尔滨工业大学 | A kind of high electric property ternary system lead titanate relaxor ferroelectric orientation ceramic of low temperature texture and its preparation method and application |
| CN110342935A (en) * | 2019-06-20 | 2019-10-18 | 广东捷成科创电子股份有限公司 | Modified lead magnesium niobate-lead titanate base piezoelectricity ferro thick-film material of a kind of Sm and preparation method thereof |
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| CN102051685A (en) * | 2009-10-28 | 2011-05-11 | 中国科学院福建物质结构研究所 | Novel ferroelectric single-crystal lead ytterbium niobate-lead magnesium niobate-lead titanate |
| CN102320831A (en) * | 2011-05-27 | 2012-01-18 | 合肥工业大学 | Zinc-bismuth based perovskite-lead titanate-lead based relaxor ferroelectric ternary system piezoceramics and preparation method thereof |
| CN102649643A (en) * | 2012-04-25 | 2012-08-29 | 中国科学院福建物质结构研究所 | Lead lutecium niobate-lead zirconate titanate piezoceramic material |
| CN102817080A (en) * | 2012-09-04 | 2012-12-12 | 中国科学院上海硅酸盐研究所 | Lead lutetioniobate-lead magnesioniobate-lead titanate ternary-system relaxation ferroelectric monocrystal and preparation method thereof |
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2012
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Patent Citations (4)
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| CN102051685A (en) * | 2009-10-28 | 2011-05-11 | 中国科学院福建物质结构研究所 | Novel ferroelectric single-crystal lead ytterbium niobate-lead magnesium niobate-lead titanate |
| CN102320831A (en) * | 2011-05-27 | 2012-01-18 | 合肥工业大学 | Zinc-bismuth based perovskite-lead titanate-lead based relaxor ferroelectric ternary system piezoceramics and preparation method thereof |
| CN102649643A (en) * | 2012-04-25 | 2012-08-29 | 中国科学院福建物质结构研究所 | Lead lutecium niobate-lead zirconate titanate piezoceramic material |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104372409A (en) * | 2013-08-14 | 2015-02-25 | 中国科学院上海硅酸盐研究所 | Ternary relaxor-based ferroelectric piezoelectric single crystal and growing method thereof |
| CN104372409B (en) * | 2013-08-14 | 2017-03-01 | 中国科学院上海硅酸盐研究所 | Ternary system relaxation base ferroelectric piezoelectric single crystal and its growing method |
| CN103641478A (en) * | 2013-11-28 | 2014-03-19 | 中国科学院福建物质结构研究所 | Ferroelectric piezoelectric ceramic material of large-power energy transducer and preparation method thereof |
| CN109650888A (en) * | 2018-12-27 | 2019-04-19 | 哈尔滨工业大学 | A kind of high electric property ternary system lead titanate relaxor ferroelectric orientation ceramic of low temperature texture and its preparation method and application |
| CN110342935A (en) * | 2019-06-20 | 2019-10-18 | 广东捷成科创电子股份有限公司 | Modified lead magnesium niobate-lead titanate base piezoelectricity ferro thick-film material of a kind of Sm and preparation method thereof |
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| CN103011815B (en) | 2017-10-24 |
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