CN103102154A - Bi0.5Na0.5TiO3-BaTiO3-BiMg0.5Ti0.5O3 lead-free piezoelectric ceramic material - Google Patents

Bi0.5Na0.5TiO3-BaTiO3-BiMg0.5Ti0.5O3 lead-free piezoelectric ceramic material Download PDF

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CN103102154A
CN103102154A CN2013100428486A CN201310042848A CN103102154A CN 103102154 A CN103102154 A CN 103102154A CN 2013100428486 A CN2013100428486 A CN 2013100428486A CN 201310042848 A CN201310042848 A CN 201310042848A CN 103102154 A CN103102154 A CN 103102154A
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朱满康
段成辉
侯育冬
刘晶冰
王如志
刘立英
汪浩
严辉
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Beijing University of Technology
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Abstract

The invention provides a Bi0.5Na0.5TiO3-BaTiO3-BiMg0.5Ti0.5O3 lead-free piezoelectric ceramic material, relates to a multicomponent system lead-free piezoelectric ceramic compound and belongs to the perovskite structure piezoelectric ceramic field. The composition provided by the invention can be expressed by a general formula of xBi0.5Na0.5TiO3-yBaTiO3-zBiMg0.5Ti0.5O3, wherein the numeric area of x, y and z is indicated by the shadow area of a ternary phase diagram (the area comprises the boundary line). The lead-free piezoelectric ceramic composition further contains oxide Bi2O3; and the content of oxide Bi2O3 is 1% of the content of Bi ions in the composition. The coercive field of the system changes with the three-component system components between 20kV/cm and 40 kV/cm; the piezoelectric coefficient d33 and the electromechanical coupling coefficient Kp are increased with the increase of the value of y in the polarizable component range; d33 is unequal from 100pC/N to 170 pC/N, while Kp is from 0.1 to 0.3. Besides, the depolarization temperature of the ceramics is slightly reduced between 80 DEG C and 120 DEG C with the increase of y.

Description

Bi 0.5Na 0.5TiO 3-BaTiO 3– BiMg 0.5Ti 0.5O 3Lead-free piezoceramic material
Technical field
The invention belongs to perovskite structure piezoelectric ceramics field, relate to the novel polynary Bi with higher pressure electrical property of a class 0.5Na 0.5TiO 3Base leadless piezoelectric ceramics material, specifically xBi 0.5Na 0.5TiO 3-yBaTiO 3-zBiMg 0.5Ti 0.5O 3Series lead-free piezoelectric ceramic.
Background technology
Piezoelectric ceramics is widely used in the fields such as ultrasonic transduction, sensor, nondestructive testing and mechanics of communication as electricity, power, heat, light sensitive material.Zirconium metatitanic acid Pb (Ti, the Zr) O that particularly has excellent piezoelectric property and high-curie temperature 3After pottery was succeeded in developing, constitutional features was ABO 3The lead-based perovskite piezoelectric ceramics development in recent years of type is very rapid, and piezoelectric filter, micro positioner, driving mechanism and sensor with it is made are widely used in the high-technology fields such as satellite broadcasting, electronics, biology and aerospace.
Present most widely used general Pb-based lanthanumdoped zirconate titanates (PbZr xTi 1-xO 3, be abbreviated as PZT) and the base pottery, be a kind of technical maturity, the perovskite structure electrical verification pottery that excellent performance is stable.Yet in the PZT material, plumbous oxide accounts for 70% left and right of raw material gross weight.Plumbous oxide is poisonous, and is volatile under high temperature, this class material preparation, use and discarded last handling process in bring infringement all can for environment and the mankind.Along with the enhancing of environment protection and human social implementation and public's environmental protection consciousness, the friendly Ferroelectric piezoelectric ceramics of research and development novel environmental has been called one of focus that World Developed Countries endeavours to research and develop.Lead-free piezoceramic material mainly contains uhligite, tungsten bronze(s) and three kinds of crystal structure types of bismuth stratiform.Wherein, the Na of perovskite structure 0.5Bi 0.5TiO 3(referred to as BNT) base piezoelectric ceramic system is that most study is also the piezoelectric ceramics system that is hopeful most to replace the PZT system.。
BNT is that year nineteen sixties is by the perovskite typed relaxation ferroelectrics of the compound replacement in a kind of A position of the people such as Smolenskii discovery.Have stronger piezoelectricity, belong to tripartite's ferroelectric phase during room temperature, the large (k of electromechanical coupling factor anisotropy tApproximately 50%, k pApproximately 13%), Curie temperature higher (320 ° of C), and sintering temperature low (＜1200 ° of C) are so become a kind of outstanding leadless piezoelectric core material.But because its piezoelectric activity is low, the large (73kVcm of coercive field -1) and specific conductivity high and be difficult to polarization, therefore be tied to form in order to improve the effective means of BNT ceramic performance by forming multivariate solid solution with other compound solid solution.(1-x) Bi in BNT based solid solution system 0.5Na 0.5TiO 3-xBaTiO 3Binary solid solution system is a kind of research piezoelectric ceramics system quite widely, and it accurate homotype phase boundary occurs at x=0.06 place, the system phase structure by tripartite's symmetrical structure (x＜0.06) to cubic symmetrical structure (x〉0.06) transformation.Has excellent piezoelectric property (d near with phase boundary in standard 33 -155pC/N).
BiMg 0.5Ti 0.5O 3(BMT) be a kind of compound of perovskite structure, pure BMT is the unsettled compound of a kind of mechanism, need to just can make in high temperature and high pressure environment.Theoretical Calculation and experiment show, this compound has and PbZrO 3Similar Symmetric Orthogonal structure joins the PbTiO of tetragonal 3The time can form equally the tripartite similar to the PZT system-cubic accurate homotype phase boundary, obtain excellent performance.Therefore at Bi 0.5Na 0.5TiO 3-BaTiO 3Thereby the generation that the cubic phase region of binary system adds a certain amount of BMT can bring out phase boundary improves the electric property of system.While BaTiO 3Be a kind of perovskite compound with high stability, energy and many uhligites form stable system solid solution, BaTiO in system 3Existence, can improve the uhligite stability of compound system, effectively suppress the generation of the dephasign that the unstable due to BMT itself causes.Empirical tests, this system piezo-electric modulus in the certain ingredients scope can reach the 170pC/N left and right, is a kind of piezoceramic material with higher pressure electrical property.
Summary of the invention
The purpose of this invention is to provide the first leadless piezoelectric ceramics system in a kind of novel B NT Quito, it is characterized in that containing the composition general formula that it is characterized in that stupalith can represent with xBNT-y BT-zBMT, and x, y, z are comprised in each composition of the ternary composition diagram of BNT-BT-BMT and put the zone (this zone comprises the boundary line) that A, a B, C and line thereof surround, and wherein A is (0.7,0.10,0.2), B is (0.9,0.1,0), C is (0.7,0.3,0).
For reaching goal of the invention, the present invention is by introducing cubic perovskite structure BaTiO 3, and BiMg 0.5Ti 0.5O 3With Bi 0.5Na 0.5TiO 3Formation ternary solid solution system is to form the accurate homotype phase boundary in tripartite four directions.The chemical formula of the leadless piezoelectric ceramics that the present invention obtains is xBi 0.5Na 0.5TiO 3-yBaTiO 3-zBiMg 0.5Ti 0.5O 3
For reaching goal of the invention, the present invention can add Bi in above-mentioned ternary solid solution is 2O 3, to reaching better effect, wherein Bi 2O 3Content increase 0.05%-1.00% on the basis of its stoichiometric ratio.
In the present invention, can add characteristic according to the purposes of piezoceramic material and regulate auxiliary agent, thereby regulate properties of materials.Regulate auxiliary agent as characteristic, preferred transition metal oxide.The example of transition metal oxide comprises Mn 2O 3, Co 2O 3, Fe 2O 3, NiO and Cr 2O 3
The present invention adopts traditional ceramic preparation technology, and described general formula is xBi 0.5Na 0.5TiO 3-yBaTiO 3-zBiMg 0.5Ti 0.5O 3The leadless piezoelectric ceramics raw material that can adopt be technical pure or chemical pure Na 2CO 3, Bi 2O 3, TiO 2, BaCO 3, MgO.Concrete preparation method's method is, according to chemical general formula and stoichiometric ratio raw materials weighing, with raw material ball milling 24 hours in ethanol, so that raw material fully mixes, in the alumina crucible of packing into after the raw material stoving that mixes, calcine soaking time 2 hours at 800-950 ° of C.The powder that calcining is synthesized is levigate through the ball milling of 12 hours again.
Adding additives in the powder of oven dry at the forming under the pressure of 120Mpa, is pressed into diameter 11.5mm, the forming composition about thickness 1.5mm.With the forming composition binder removal, sintering 2 hours under 1100-1200 ° of C at last, the ceramic plate after sintering is by upper silver electrode, in the silicone oil of 50 ° of C, at 5kVmm -1Voltage under the 30-60min that polarizes.Then sample is carried out the test of properties.
The present invention has realized successfully that by the structure of BNT base ternary solid solution system coercive field is at 20-50kVcm to the improvement of BNT based leadless piezoelectric ceramics properties -1Between change along with the variation of ternary system component, ceramic composition is (due to the generation that antiferroelectric phase is brought out in membership that adds of BMT, some component can't polarize) piezoelectric coefficient d in polarizable scope 33With electromechanical coupling factor k pIncrease d along with the increase of z value 33At 100-170pCN -1In do not wait, and K pDo not wait in 0.1-0.3.
Description of drawings
Fig. 1 is xBi of the present invention 0.5Na 0.5TiO 3-yBaTiO 3-zBiMg 0.5Ti 0.5O 3The ternary phase diagrams of system piezoelectric ceramics, dash area is composition range involved in the present invention, this zone comprises the line segment between an A and D, also comprise the line segment between a B and C, but do not comprise the some A of an A and B and the line segment between B, do not comprise the some C of a C and D and the line segment between D yet.
Fig. 2 is that composition of the present invention consists of x=0.8575, and y=0.1225, z=0.02 are 0.8575Bi 0.5Na 0.5TiO 3– 0.1225BaTiO 3– 0.02BiMg 0.5Ti 0.5O 3The time ferroelectric hysteresis loop.
Embodiment
Below will describe the present invention by embodiment, these embodiment are the purpose of property explanation presented for purpose of illustration just, but not is used for limiting the present invention.
Preparing general formula of the present invention is xBi 0.5Na 0.5TiO 3-yBaTiO 3– zBiMg 0.5Ti 0.5O 3Leadless piezoelectric ceramics can adopt technical pure or chemical pure Na 2CO 3, Bi 2O 3, TiO 2, BaCO 3, MgO is raw material, makes according to traditional ceramic preparation technology.Concrete preparation method is, according to chemical general formula and stoichiometric ratio raw materials weighing, with raw material ball milling 24 hours in ethanol, so that raw material fully mixes, in the alumina crucible of packing into after the raw material stoving that mixes, calcine soaking time 2 hours at 800-950 ° of C.The powder that calcining is synthesized is levigate through the ball milling of 12 hours again.
Adding additives in the powder of oven dry at the forming under the pressure of 120Mpa, is pressed into diameter 11.5mm, the forming composition about thickness 1.5mm.With the forming composition binder removal, sintering 2 hours under 1100-1200 ° of C at last, the ceramic plate after sintering is by upper silver electrode, in the silicone oil of 50 ° of C, at 5kVmm -1Voltage under the 30-60min that polarizes.Then sample is carried out the test of properties.
Formula and the performance of the leadless piezoelectric ceramics of preparation are as follows according to the method described above:
Embodiment 1:
Formula:
0.9Bi 0.5Na 0.5TiO 3-0.1BaTiO 3-0BiMg 0.5Ti 0.5O 3
Technique: 850 ° of C of calcining temperature, 1200 ° of C of sintering temperature.
Embodiment 2:
Formula:
0.7Bi 0.5Na 0.5TiO 3-0.30BaTiO 3-0BiMg 0.5Ti 0.5O 3
Technique: 900 ° of C of calcining temperature, 1100 ° of C of sintering temperature.
Embodiment 3:
Formula:
0.7Bi 0.5Na 0.5TiO 3-0.1BaTiO 3-0.2BiMg 0.5Ti 0.5O 3
Technique: 850 ° of C of calcining temperature, 1150 ° of C of sintering temperature.
Embodiment 4:
Formula:
0.8575Bi 0.5Na 0.5TiO 3-0.1225BaTiO 3-0.02BiMg 0.5Ti 0.5O 3
Technique: 900 ° of C of calcining temperature, 1175 ° of C of sintering temperature.
Each embodiment performance table:
Figure BDA00002812468100041
Annotate: can't polarize with the appearance of * component due to antiferroelectric phase.

Claims (3)

1.Bi 0.5Na 0.5TiO 3-BaTiO 3– BiMg 0.5Ti 0.5O 3Lead-free piezoceramic material is characterized in that containing three kinds of compositions of BNT, BT and BMT, and wherein, BNT is Bi 0.5Na 0.5TiO 3, BT is BaTiO 3, BMT is BiMg 0.5Ti 0.5O 3The composition general formula of stupalith represents with x BNT-y BT-z BMT, and x, y, z is comprised in each composition of the ternary composition diagram of BNT-BT-BMT and puts the zone that A, a B, C and line thereof surround, and this zone comprises the boundary line, and wherein A is (0.7,0.10,0.2), B is (0.9,0.1,0), C is (0.7,0.3,0).
2. lead-free piezoceramic material as claimed in claim 1, is characterized in that system has the crystalline structure of cubic uhligite crystalline phase.
3. lead-free piezoceramic material as claimed in claim 1, wherein Bi 2O 3Content increase 0.05%-1.00% on the basis of its stoichiometric ratio.
CN201310042848.6A 2013-02-03 2013-02-03 Bi0.5Na0.5TiO3-BaTiO3-BiMg0.5Ti0.5O3 lead-free piezoelectric ceramic material Expired - Fee Related CN103102154B (en)

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Cited By (12)

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CN103482973A (en) * 2013-09-10 2014-01-01 天津大学 Lead-free quaternary system electro-strain piezoelectric ceramic material, preparation method and product
CN103803966A (en) * 2013-12-19 2014-05-21 桂林电子科技大学 High-temperature leadless piezoelectric ceramic with near-zero temperature coefficient and preparation method thereof
CN104628380A (en) * 2013-11-13 2015-05-20 Tdk株式会社 Piezoelectric composition and piezoelectric element
CN105859283A (en) * 2016-05-06 2016-08-17 北京工业大学 K0.5Bi0.5TiO3-BiNi0.5Zr0.5O3 electrostrictive ceramic material and preparation thereof
CN106977195A (en) * 2017-03-20 2017-07-25 北京工业大学 It is a kind of to have without the BNT base ternary lead-free ferroelectric ceramics of delayed big electric field induced strain and preparation
CN107721411A (en) * 2017-11-03 2018-02-23 北京工业大学 A kind of unleaded BNT BT matrixes system of big electric field induced strain
CN108929111A (en) * 2018-09-10 2018-12-04 武汉理工大学 A kind of dielectric film and preparation method thereof of superelevation discharge energy-storage density
CN110312692A (en) * 2017-02-03 2019-10-08 赛尔科技有限公司 Ceramic material, preparation method and use comprising counterfeit cubic phase
CN110498679A (en) * 2019-09-27 2019-11-26 哈尔滨理工大学 A kind of preparation method of high dielectric property multilayer phase structure BNT-BT ceramics
CN112062555A (en) * 2020-09-17 2020-12-11 广西大学 Preparation method of BNT-BT-based lead-free negative electricity card material by doping induction of functional groups
CN113999004A (en) * 2021-11-08 2022-02-01 西安电子科技大学 Lead-free high-energy-storage-density ceramic material and preparation method thereof
CN115010483A (en) * 2022-06-29 2022-09-06 西安交通大学 Piezoelectric ceramic material insensitive to strain and components and preparation method and application thereof

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Cited By (19)

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Publication number Priority date Publication date Assignee Title
CN103482973A (en) * 2013-09-10 2014-01-01 天津大学 Lead-free quaternary system electro-strain piezoelectric ceramic material, preparation method and product
CN104628380A (en) * 2013-11-13 2015-05-20 Tdk株式会社 Piezoelectric composition and piezoelectric element
CN103803966A (en) * 2013-12-19 2014-05-21 桂林电子科技大学 High-temperature leadless piezoelectric ceramic with near-zero temperature coefficient and preparation method thereof
CN105859283A (en) * 2016-05-06 2016-08-17 北京工业大学 K0.5Bi0.5TiO3-BiNi0.5Zr0.5O3 electrostrictive ceramic material and preparation thereof
CN105859283B (en) * 2016-05-06 2019-03-22 北京工业大学 K0.5Bi0.5TiO3–BiNi0.5Zr0.5O3Electrostriction ceramics material and preparation
CN110312692A (en) * 2017-02-03 2019-10-08 赛尔科技有限公司 Ceramic material, preparation method and use comprising counterfeit cubic phase
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CN106977195A (en) * 2017-03-20 2017-07-25 北京工业大学 It is a kind of to have without the BNT base ternary lead-free ferroelectric ceramics of delayed big electric field induced strain and preparation
CN107721411B (en) * 2017-11-03 2020-11-20 北京工业大学 Lead-free BNT-BT matrix ceramic with large electrostriction
CN107721411A (en) * 2017-11-03 2018-02-23 北京工业大学 A kind of unleaded BNT BT matrixes system of big electric field induced strain
CN108929111B (en) * 2018-09-10 2021-06-22 武汉理工大学 Dielectric film with ultrahigh discharge energy storage density and preparation method thereof
CN108929111A (en) * 2018-09-10 2018-12-04 武汉理工大学 A kind of dielectric film and preparation method thereof of superelevation discharge energy-storage density
CN110498679A (en) * 2019-09-27 2019-11-26 哈尔滨理工大学 A kind of preparation method of high dielectric property multilayer phase structure BNT-BT ceramics
CN110498679B (en) * 2019-09-27 2021-12-14 哈尔滨理工大学 Preparation method of multilayer phase structure BNT-BT ceramic with high dielectric property
CN112062555A (en) * 2020-09-17 2020-12-11 广西大学 Preparation method of BNT-BT-based lead-free negative electricity card material by doping induction of functional groups
CN113999004A (en) * 2021-11-08 2022-02-01 西安电子科技大学 Lead-free high-energy-storage-density ceramic material and preparation method thereof
CN115010483A (en) * 2022-06-29 2022-09-06 西安交通大学 Piezoelectric ceramic material insensitive to strain and components and preparation method and application thereof
CN115010483B (en) * 2022-06-29 2023-06-16 西安交通大学 Piezoelectric ceramic material insensitive to strain and components, and preparation method and application thereof

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