CN105732024A - Novel binary K0.5Bi0.5TiO3-BiMg0.5Zr0.5O3 leadless piezoelectric ceramic material and preparation - Google Patents

Novel binary K0.5Bi0.5TiO3-BiMg0.5Zr0.5O3 leadless piezoelectric ceramic material and preparation Download PDF

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CN105732024A
CN105732024A CN201610035194.8A CN201610035194A CN105732024A CN 105732024 A CN105732024 A CN 105732024A CN 201610035194 A CN201610035194 A CN 201610035194A CN 105732024 A CN105732024 A CN 105732024A
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tio
piezoelectric ceramics
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朱满康
胡彬彬
郭金键
郑木鹏
侯育冬
刘晶冰
王如志
汪浩
严辉
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Beijing University of Technology
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Abstract

The invention discloses a novel binary K0.5Bi0.5TiO3-BiMg0.5Zr0.5O3 leadless piezoelectric ceramic material and preparation, and belongs to the field of piezoelectric ceramic of a perovskite structure. The material is expressed in a general formula (1-x)K0.5Bi0.5TiO3-xBiMg0.5Zr0.5O3 (x is greater than 0 and less than or equal to 0.08). The calcination temperature of the system is 800-900 DEG C, the briquetting pressure of the system is 150-300MPa, and the sintering temperature of the system is 1040-1080 DEG C. Improvement on piezoelectric properties of the KBT leadless piezoelectric ceramic material is successfully achieved, and near a morphotropic phase boundary, x is equal to 0.01, that is, the maximum d33=65pC/N can be achieved when composition is 0.99K0.5Bi0.5TiO3-0.01BiMg0.5Zr0.5O3.

Description

Novel Dual system K0.5Bi0.5TiO3–BiMg0.5Zr0.5O3Lead-free piezoceramic material and Preparation
Technical field
The invention belongs to perovskite structure piezoelectric ceramics field, relate to the binary with higher pressure electrical property that a class is novel K0.5Bi0.5TiO3Base leadless piezoelectric ceramics material, specifically (1-x) K0.5Bi0.5TiO3-xBiMg0.5Zr0.5O3(0<x≤0.08) Series lead-free piezoelectric ceramic material composition and preparation method thereof.
Technical background
Piezoelectric ceramics refers to have piezoelectric effect, it is possible to by a kind of ceramic material of mutual to mechanical energy and electric energy phase transformation. As a kind of electron ceramic material, it is widely used for preparing the electronics unit devices such as sensor, piezoelectric transducer, piezoelectric actuator Part, application is quite varied, and the life with us is closely bound up.Particularly there is excellent piezoelectric property and high-curie temperature Lead zirconate titanate Pb (Ti, Zr) O3After pottery is succeeded in developing, architectural feature is ABO3The lead-based perovskite piezoelectric ceramics of type develops very Rapidly, piezoelectric filter, micro positioner, driver and the sensor etc. made of it, it is widely used in satellite broadcasting, electronics The high-technology fields such as equipment, biology and Aero-Space.
Current most widely used lead zirconate titanate (PbZrxTi1-xO3, be abbreviated as PZT) base pottery, be a kind of technical maturity, The perovskite structure piezoelectric ceramics that excellent performance is stable.But, PbO in lead base piezoelectric ceramics (or Pb3O4) content to account for raw material total More than the 70% of amount, the lead of such high-load is prepared at piezoelectric ceramics, is used, it is ecological all to give in waste treatment or removal process Environment and the mankind cause serious harm.Along with various circles of society's attention to environmental protection problem, a lot of countries propose decree one after another Regulation forbid the use of leaded piezoelectricity ferro material, environmentally friendly unleaded foundary weight electroceramics become various countries endeavour research and development and One of important materials paid close attention to.
Lead-free piezoceramic material mainly has perovskite, tungsten bronze and three kinds of crystal structure types of bismuth stratiform.Wherein, calcium titanium Ore deposit structure Na0.5Bi0.5TiO3(referred to as BNT) matrix system is the leadless piezoelectric system that research is more.But the pole of simple NBT pottery Changing the most difficult, there is relatively low depolarization temperature, and be difficult to eliminate, this most seriously limits its actual application.KBT is i.e. K0.5Bi0.5TiO3, it is Tetragonal under room temperature, quite similar with NBT, also it is a kind of ABO3The ferroelectric material of type perovskite structure, with NBT compares, and KBT has higher Curie temperature (TC=380 DEG C) and relatively low coercive field (Ec=15kV/cm), and do not exist and move back pole Change temperature, there is broader practice prospect.By the multivariate solid solution system being compounded to form with other perovskite structure compound, Sintering and the electric property of KBT pottery can be improved further.
BiMg0.5Zr0.5O3(BMZ) it is a kind of compound with metastable perovskite-like structure, it is difficult to synthesis.BMZ has There is the relatively low tolerance factor, be incorporated into the K of tetragonal0.5Bi0.5TiO3In may form quasi-homotype phase boundary therewith.Therefore, by The binary system piezoelectric ceramics that KBT-BMZ is constituted, is likely to be of good piezoelectric property.
Summary of the invention
It is an object of the invention to provide a kind of novel KBT base binary leadless piezoelectric ceramics system.
One KBT base binary leadless piezoelectric ceramics system of the present invention, it is characterised in that KBT base binary leadless piezoelectric ceramics System contains two kinds of compositions of KBT, BMZ, and wherein, KBT is K0.5Bi0.5TiO3, BMZ is BiMg0.5Zr0.5O3；The formula of composition represents For (1-x) K0.5Bi0.5TiO3-xBiMg0.5Zr0.5O3(0<x≤0.08)。
The present invention uses BiMg0.5Zr0.5O3With K0.5Bi0.5TiO3Constitute binary solid solution system, formed and there is cubic perovskite The quasi-homotype phase boundary coexisted with counterfeit cubic perovskite phase crystal structure mutually.The chemical general formula of the leadless piezoelectric ceramics that the present invention obtains For (1-x) K0.5Bi0.5TiO3-xBiMg0.5Zr0.5O3(0 < x≤0.08, preferably 0.01).
The present invention uses traditional ceramic preparation technology, and described formula is (1-x) K0.5Bi0.5TiO3-xBiMg0.5Zr0.5O3 Leadless piezoelectric ceramics use raw material be mainly chemical pure or electron level K2CO3、Bi2O3、TiO2、ZrO2、4MgCO3·Mg (OH)2·5H2O etc..Concrete preparation method is, measures ratio according to the chemistry mole of chemical general formula and weighs raw material, by raw material at ethanol Middle ball milling 12 hours, so that raw material is sufficiently mixed uniformly, will load in alumina crucible after the raw material stoving of mix homogeneously, Calcine for 800 DEG C-900 DEG C, temperature retention time 3 hours.The powder of calcining synthesis is levigate through the ball milling of 12 hours again；By ball milling Levigate powder dries then adding additives, at the forming under the pressure of 150MPa-300MPa, then by article shaped binder removal, finally Sinter 4 hours at 1040 DEG C-1080 DEG C, obtain leadless piezoelectric ceramics system.
Potsherd after sintering is by upper silver electrode, in the silicone oil of 120 DEG C, at 4.5kV mm-1Voltage under polarize 30min.Then sample is carried out the test of properties.
The present invention, by the structure of KBT base binary solid solution system, is successfully realized KBT leadless piezoelectric ceramics piezoelectric property Improvement, this system coercive field changes, piezoelectricity system along with the change of binary system component between 17kV/cm～31kV/cm Number d33From 17pC/N～65pC/N, near quasi-homotype phase boundary, x=0.01 i.e. component is 0.99K0.5Bi0.5TiO3- 0.01BiMg0.5Zr0.5O3Time have maximum d33=65pC/N.
Accompanying drawing explanation
Fig. 1 be the chemical composition of the present invention be 0.99K0.5Bi0.5TiO3-0.01BiMg0.5Zr0.5O3, i.e. during x=0.01 Ferroelectric hysteresis loop；
The chemical composition of Fig. 2 present invention is 0.99K0.5Bi0.5TiO3-0.01BiMg0.5Zr0.5O3The X of 44 °～48 ° scopes The diffraction maximum of ray diffraction spectra, the tetragonal that can substantially where there is and cubic structure.
Detailed description of the invention
Hereinafter will be described the present invention by embodiment, these embodiments are simply for the mesh of exemplary illustration , not for limiting the present invention.
Preparing formula of the present invention is (1-x) K0.5Bi0.5TiO3-xBiMg0.5Zr0.5O3(0 < x≤0.08) unleaded Piezoelectric ceramics, can use chemical pure or electron level K2CO3, Bi2O3, TiO2, ZrO2, 4MgCO3·Mg(OH)2·5H2O etc. are for former Material, prepares according to traditional ceramic preparation technology.Concrete preparation method is, weighs former according to chemical general formula and stoichiometric proportion Material, by raw material ball milling 12 hours in ethanol, so that raw material is sufficiently mixed uniformly, will load oxygen after the raw material stoving of mix homogeneously Change in aluminum crucible, calcine at 800 DEG C-900 DEG C, temperature retention time 3 hours.The powder of calcining synthesis is again through the ball of 12 hours Grind levigate.
Adding additives after the powder drying that ball milling is levigate, at the forming under the pressure of 150MPa-300Mpa, is pressed into diameter 11.5mm, the article shaped of thickness about 1.5mm.By article shaped binder removal, finally sinter 4 hours at 1040 DEG C-1080 DEG C, sintering After potsherd by upper silver electrode, in the silicone oil of 120 DEG C, at 4.5kV mm-1Voltage under polarize 30min.Then to sample Carry out the test of properties.
Formula and the performance of the leadless piezoelectric ceramics prepared according to the method described above are as follows:
Comparative example:
Formula:
K0.5Bi0.5TiO3
Technique:
According to K0.5Bi0.5TiO3Formula weigh raw material, by raw material ball milling 12 hours in ethanol, former by mix homogeneously Material loads in alumina crucible after drying, and calcines at 800 DEG C, temperature retention time 3 hours.The powder of calcining synthesis is again through 12 Hour ball milling levigate.Adding additives in the powder dried, at the forming under the pressure of 150MPa, is pressed into diameter 11.5mm, The article shaped of thickness about 1.5mm.By article shaped binder removal, finally sinter 4 hours at 1040 DEG C.
Embodiment 1:
Formula:
0.99K0.5Bi0.5TiO3-0.01BiMg0.5Zr0.5O3
Technique: according to 0.99K0.5Bi0.5TiO3-0.01BiMg0.5Zr0.5O3Formula weigh raw material, calcining heat 830 DEG C, Briquetting pressure is 190MPa, sintering temperature 1050 DEG C；Other process conditions are identical with comparative example.
Embodiment 2:
Formula:
0.97K0.5Bi0.5TiO3-0.03BiMg0.5Zr0.5O3
Technique: according to 0.97K0.5Bi0.5TiO3-0.03BiMg0.5Zr0.5O3Formula weigh raw material, calcining heat 855 DEG C, Briquetting pressure is 230MPa, sintering temperature 1060 DEG C；Other process conditions are identical with comparative example.
Embodiment 3:
Formula:
0.95K0.5Bi0.5TiO3-0.05BiMg0.5Zr0.5O3
Technique: according to 0.95K0.5Bi0.5TiO3-0.05BiMg0.5Zr0.5O3Formula weigh raw material calcining heat 870 DEG C, Briquetting pressure is 270MPa, sintering temperature 1070 DEG C；Other process conditions are identical with comparative example.
Embodiment 4:
Formula:
0.92K0.5Bi0.5TiO3-0.08BiMg0.5Zr0.5O3
Technique: according to 0.92K0.5Bi0.5TiO3-0.08BiMg0.5Zr0.5O3Formula weigh raw material calcining heat 900 DEG C, Briquetting pressure is 300MPa, sintering temperature 1080 DEG C；Other process conditions are identical with comparative example.
Table 1 each embodiment performance table:

Claims (4)

1. a KBT base binary leadless piezoelectric ceramics system, it is characterised in that KBT base binary leadless piezoelectric ceramics system contains Two kinds of compositions of KBT, BMZ, wherein, KBT is K0.5Bi0.5TiO3, BMZ is BiMg0.5Zr0.5O3；The formula of composition is (1-x) K0.5Bi0.5TiO3-xBiMg0.5Zr0.5O3, 0 < x≤0.08.
2. according to a kind of KBT base binary leadless piezoelectric ceramics system described in claim 1, it is characterised in that x=0.01.
3. according to a kind of KBT base binary leadless piezoelectric ceramics system described in claim 1 or 2, it is characterised in that BiMg0.5Zr0.5O3With K0.5Bi0.5TiO3Form binary solid solution system, formed and there is cubic Perovskite Phase and counterfeit cubic perovskite phase The quasi-homotype phase boundary that crystal structure coexists.
4. the method preparing KBT base binary leadless piezoelectric ceramics system described in any one of claim 1-3, its feature exists In, raw material is mainly chemical pure or electron level K2CO3、Bi2O3、TiO2、ZrO2、4MgCO3·Mg(OH)2·5H2O, specifically prepares Method is: measures ratio according to the chemistry mole of chemical general formula and weighs raw material, by raw material ball milling 12 hours in ethanol, so that raw material It is sufficiently mixed uniformly, by loading in alumina crucible after the raw material stoving of mix homogeneously, calcines at 800 DEG C-900 DEG C, protect The 3 hours time of temperature.The powder of calcining synthesis is levigate through the ball milling of 12 hours again；Then powder drying levigate for ball milling is added viscous Knot agent, at the forming under the pressure of 150MPa-300MPa, then by article shaped binder removal, finally sinters 4 at 1040 DEG C-1080 DEG C Hour, obtain KBT base binary leadless piezoelectric ceramics system.
CN201610035194.8A 2016-01-19 2016-01-19 Novel Dual system K0.5Bi0.5TiO3–BiMg0.5Zr0.5O3Lead-free piezoceramic material and preparation Expired - Fee Related CN105732024B (en)

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CN107892567A (en) * 2017-11-03 2018-04-10 北京工业大学 One kind (Bi1/2K1/2)TiO3Base binary leadless piezoelectric ceramics and its preparation
CN109180180A (en) * 2018-10-25 2019-01-11 北京工业大学 The preparation method of one step pressureless sintering synthesizing submicron crystalline substance scale piezoceramic material
CN115849901A (en) * 2022-12-03 2023-03-28 北京工业大学 K 0.5 Bi 0.5 TiO 3 Base ternary system dielectric energy storage lead-free ceramic material

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107892567A (en) * 2017-11-03 2018-04-10 北京工业大学 One kind (Bi1/2K1/2)TiO3Base binary leadless piezoelectric ceramics and its preparation
CN107892567B (en) * 2017-11-03 2020-12-04 北京工业大学 (Bi)1/2K1/2)TiO3Base binary leadless piezoelectric ceramic and preparation thereof
CN109180180A (en) * 2018-10-25 2019-01-11 北京工业大学 The preparation method of one step pressureless sintering synthesizing submicron crystalline substance scale piezoceramic material
CN109180180B (en) * 2018-10-25 2021-07-02 北京工业大学 Preparation method for synthesizing piezoelectric ceramic material with submicron crystal size by one-step pressureless sintering
CN115849901A (en) * 2022-12-03 2023-03-28 北京工业大学 K 0.5 Bi 0.5 TiO 3 Base ternary system dielectric energy storage lead-free ceramic material
CN115849901B (en) * 2022-12-03 2023-08-18 北京工业大学 K (K) 0.5 Bi 0.5 TiO 3 Basic ternary system dielectric energy storage lead-free ceramic material

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