CN106518058B - A kind of unleaded compound ferroelectric ceramics being made of bismuth potassium titanate and zinc oxide and preparation - Google Patents

A kind of unleaded compound ferroelectric ceramics being made of bismuth potassium titanate and zinc oxide and preparation Download PDF

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CN106518058B
CN106518058B CN201610968638.3A CN201610968638A CN106518058B CN 106518058 B CN106518058 B CN 106518058B CN 201610968638 A CN201610968638 A CN 201610968638A CN 106518058 B CN106518058 B CN 106518058B
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朱满康
李玲
位秋梅
郑木鹏
侯育冬
汪浩
严辉
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Beijing University of Technology
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Abstract

A kind of unleaded compound ferroelectric ceramics being made of bismuth potassium titanate and zinc oxide and preparation, belong to ferroelectric ceramics technical field.In order to inhibit K0.5Bi0.5TiO3Depolarization phenomenon, improve ferroelectric properties, with K2CO3、TiO2、Bi2O3And ZnO is raw material, passes through two step Solid phase synthesis non-plumbum ferroelectric composite ceramics K0.5Bi0.5TiO3:ZnO.By X-ray diffraction, scanning electron microscope and measurement, the microstructure and Dielectric behavior of composite ceramics are analyzed.The result shows that: K0.5Bi0.5TiO3Third phase Zn is generated after middle ZnO, in composite ceramics2TiO4, the introducing of ZnO inhibits K0.5Bi0.5TiO3From normal frroelectrics to the phase transition of relaxation ferroelectric, to K0.5Bi0.5TiO3Application and research have important role.

Description

A kind of unleaded compound ferroelectric ceramics being made of bismuth potassium titanate and zinc oxide and preparation
Technical field
The present invention relates to a kind of novel K0.5Bi0.5TiO3: the unleaded compound ferroelectric ceramics of ZnO, is by Ca-Ti ore type K0.5Bi0.5TiO3It is combined with Nano semiconductor ZnO, avoids being changed into relaxor ferroelectric by normal frroelectrics before curie point Body, the temperature stability with high ferroelectric properties, belongs to ferroelectric ceramics technical field.
Technical background
Piezoelectric ceramics is a kind of material to electricity, power, heat, photaesthesia, is the product that artificial polarization is carried out to ferroelectric ceramics, It has been widely applied in fields such as ultrasonic transduction, sensor, non-destructive testing and communications.Ferroelectric ceramics general at present is with Pb (Zr,Ti)O3(PZT) based on ceramics, wherein lead content is volatile when at high temperature and using generally all 70% or more, is making It is standby, use and discard in last handling process and all can bring damage to environment and the mankind.The developed countries such as the U.S., Japan and European Union are Through the manufacture and use for limiting leaded ceramics by legislative pattern.It is mesh that searching, which can substitute the lead-free piezoceramic material of PZT, Urgent one of the project of preceding field of electronic materials.
Lead-free ferroelectric ceramics refer to that existing good environment harmony has a kind of new function ceramics of preferable usability again Material.The main leadless piezoelectric ceramics system studied at present has barium titanate (BaTiO3, BT) and based leadless piezoelectric ceramics, bismuth-sodium titanate (Na0.5Bi0.5TiO3, NBT) and based leadless piezoelectric ceramics, bismuth potassium titanate (K0.5Bi0.5TiO3, KBT) and based leadless piezoelectric ceramics and niobic acid Potassium sodium (Na0.5K0.5NbO3, KNN) based leadless piezoelectric ceramics etc..Wherein, perovskite structure K0.5Bi0.5TiO3(referred to as KBT) is Nineteen sixties year, when room temperature belonged to four by a kind of A complex perovskite structure ferroelectrics of the discoveries such as Smolenskii Square ferroelectric phase, Curie temperature is higher (410 DEG C), and sintering temperature is low (< 1100 DEG C), more with studying at present Na0.5Bi0.5TiO3(referred to as BNT) structure is quite similar.Compared with BNT, KBT have higher Curie temperature and it is lower rectify Stupid field ECThere is broader temperature to use section and lower polarization difficulty by=1.5kV/mm, therefore, KBT, become a kind of outstanding Lead-free ferroelectric material.By the multivariate solid solution system being compounded to form with it, it can further improve the sintering and electricity of KBT ceramics Performance.But at high temperature, KBT is a cube paraelectric phase, and when cooling to 380 DEG C, system turns generation cube-tetragonal phase Become.At T=300 DEG C, the second phase transition occurs, and nearby has the presence of thermal hysteresis at 270 DEG C.This transformation and NBT Phase transition be equally people's bone of contention, also limit the application range and temperature stability of KBT matrix system.
In dielectric and piezoelectric ceramics, ZnO is widely used as a kind of sintering aid, its addition promotes liquid phase It is formed, leads to a large amount of Ion transfer during the sintering process, to improve the compactness of ceramics, promoted crystal grain and grow up.It grinds Study carefully and shows Zn2+The electricity of ferroelectric ceramics is improved to change the temperature of phase transition in the position B that can be substituted in perovskite structure Performance.Zn2+Substitution improve ternary solid solution PbMg1/3Nb2/3O3-PbZn1/3Nb2/3O3-PbTiO3The calcium titanium of system The stability of mineral phase structure.
ZnO is introduced among KBT, a kind of composite material is formed.Using the characteristic of semiconductor of ZnO, ZnO is formed by built-in Electric field inhibits the degradation phenomena of KBT, improves the stability of phase structure.This solves a weight of the KBT before application on scape Big problem establishes solid foundation for the application development of KBT.
Summary of the invention
The purpose of the present invention is by K0.5Bi0.5TiO3With compound, the inhibition K of semiconductor ZnO0.5Bi0.5TiO3By normal Ferroelectric is changed into the phase transition of relaxation ferroelectric, improves K0.5Bi0.5TiO3The stable type of phase structure.
To reach goal of the invention, the present invention enters K by introducing nano-ZnO0.5Bi0.5TiO3In, to be formed K0.5Bi0.5TiO3: ZnO composite ceramics, to get a desired effect, wherein the molar content of ZnO is 20%~30%.
One kind is by K0.5Bi0.5TiO3The unleaded compound ferroelectric ceramics constituted with ZnO, which is characterized in that by perovskite structure K0.5Bi0.5TiO3With crystal structure made of nanoscale ZnO semiconductors coupling, general formula is (1-x) K0.5Bi0.5TiO3: XZnO, 0.20≤x≤0.30.
K0.5Bi0.5TiO3For with cubic perovskite crystal phase K0.5Bi0.5TiO3, ZnO is buergerite phase ZnO.
It is of the invention by K0.5Bi0.5TiO3With the preparation method of the ZnO unleaded compound ferroelectric ceramics constituted, feature exists In using the preparation process of two step solid phase methods, the first step is the stable K of preparation structure0.5Bi0.5TiO3Ceramic powder, second step To introduce ZnO, with K0.5Bi0.5TiO3Form composite ceramics.
K0.5Bi0.5TiO3The preparation process of ceramic powder is as follows: according to K0.5Bi0.5TiO3Element metering than weigh raw material K2CO3, Bi2O3, TiO2, the ball milling at least 12h in dehydrated alcohol is so that raw material is sufficiently mixed uniformly, after drying, 800 DEG C~ 2~5h is calcined at 850 DEG C, ball milling 12h keeps powder levigate again, and drying obtains pure perovskite phase structure K0.5Bi0.5TiO3Powder Body.To improve K0.5Bi0.5TiO3Phase stability, will the obtained K of calcining0.5Bi0.5TiO3Powder is in 980 DEG C~1020 DEG C pre-burnings 2~4h of knot is used for K through ball milling at least 12h, drying0.5Bi0.5TiO3: the preparation of ZnO composite ceramics.
K0.5Bi0.5TiO3: the preparation process of ZnO composite ceramics is as follows: pressing general formula (1-x) K0.5Bi0.5TiO3:xZnO(0.20 ≤ x≤0.30) molar ratio, weigh be pre-sintered obtain K0.5Bi0.5TiO3Powder and ZnO nano powder, ball milling at least 12h, Drying, mix adhesive PVB, compression moulding, green body after 650 DEG C of dumpings, with the rate of 3 DEG C/min be warming up to 1000 DEG C~ 1050 DEG C are sintered, and keep the temperature 1~3h, obtain K0.5Bi0.5TiO3: ZnO complex phase ceramic.It is preferred that be sintered at 1020 DEG C, Heat preservation 1.5 hours.
Sintered potsherd is by upper silver electrode, for carrying out the test of properties to sample.
Further, showing: K0.5Bi0.5TiO3After the middle ZnO for introducing 20% (mole percent), generated in composite ceramics Third phase Zn2TiO4, in particular, the introducing of ZnO inhibits K0.5Bi0.5TiO3Turn from normal frroelectrics to the phase of relaxation ferroelectric Become, to K0.5Bi0.5TiO3Application and research have important role.
The present invention passes through building K0.5Bi0.5TiO3With the 0-3 type structure of ZnO, it is successfully realized to K0.5Bi0.5TiO3Base without The improvement of galvanized iron electroceramics properties, it is suppressed that K0.5Bi0.5TiO3From normal frroelectrics to the phase transition of relaxation ferroelectric.
Detailed description of the invention
Using the phase structure of German Bruker company D8-Advance type X-ray diffractometer measurement sample, Hitachi S- 4800 scanning electron microscope measure the microstructure of material prepared.Using ferroelectricity tester (Premier II, Radiant Technologies, USA), test ferroelectric properties.Using equipped with temperature heating unit accurate LCR table (E4980, Agilent, USA) the dielectric property of test sample.
Fig. 1 is that the embodiment of the present invention 5 calcines 4h, 1000 DEG C of pre-sinterings 3h, (1- of 1020 DEG C of sintering 1.5h at 800 DEG C x)K0.5Bi0.5TiO3: the scanning electron microscope (SEM) photograph of xZnO (x=0 and 0.2)
Fig. 2 is that the embodiment of the present invention 5 calcines 4h at 800 DEG C, 1000 DEG C of pre-sinterings 3h, sintering 1.5h at 1020 DEG C (1-x)K0.5Bi0.5TiO3: the XRD spectrum of xZnO (x=0 and 0.2).
Fig. 3 is that the embodiment of the present invention 5 calcines 4h at 800 DEG C, 1000 DEG C of pre-sinterings 3h, sintering 1.5h at 1020 DEG C (1-x)K0.5Bi0.5TiO3: the dielectric thermogram of xZnO (x=0 and 0.2).
Specific embodiment
Below with reference to embodiment, the present invention will be further described, but the present invention is not limited to following embodiments.
Embodiment 1
Formula: 0.8K0.5Bi0.5TiO3:0.2ZnO
K0.5Bi0.5TiO3The preparation of powder is to analyze pure K2CO3(99.99%), Na2CO3(99.99%) and Bi2O3 It (99.99%) is raw material, according to K0.5Bi0.5TiO3Element metering than weigh raw material, in dehydrated alcohol ball milling 12h, drying Afterwards, 2h is calcined at 800 DEG C, ball milling 12h, drying, obtain pure perovskite phase structure K again0.5Bi0.5TiO3Powder.To improve K0.5Bi0.5TiO3Phase stability, will the obtained K of calcining0.5Bi0.5TiO3Powder through ball milling 12h, is dried in 980 DEG C of pre-sintering 2h It is dry, it is used for K0.5Bi0.5TiO3: the preparation of ZnO complex phase ceramic.
0.8K0.5Bi0.5TiO3: the preparation of 0.2ZnO complex phase ceramic sample weighs in molar ratio is pre-sintered acquisition K0.5Bi0.5TiO3Powder and ZnO nano powder (partial size about 30nm), ball milling 12h, drying mix adhesive PVB, in 400MPa Pressure under be pressed into diameter be 11.5mm disk.Green body is warming up to 1000 after 650 DEG C of dumpings, with the rate of 3 DEG C/min It DEG C is sintered, keeps the temperature 1h, obtain 0.8K0.5Bi0.5TiO3: 0.2ZnO complex phase ceramic.
Embodiment 2
Formula: 0.75K0.5Bi0.5TiO3:0.25ZnO
K0.5Bi0.5TiO3Powder calcination temperature is 840 DEG C, keeps the temperature 4h, and calcined temperature is 1010 DEG C, keeps the temperature 3h, K0.5Bi0.5TiO3: the sintering temperature of ZnO complex phase ceramic is 1030 DEG C, keeps the temperature 2h.The other the same as in Example 1.
Embodiment 3
Formula: 0.75K0.5Bi0.5TiO3:0.25ZnO
K0.5Bi0.5TiO3Powder calcination temperature is 820 DEG C, keeps the temperature 3h, and calcined temperature is 1000 DEG C, keeps the temperature 2.5h, K0.5Bi0.5TiO3: the sintering temperature of ZnO complex phase ceramic is 1020 DEG C, keeps the temperature 2.5h.The other the same as in Example 1.
Embodiment 4
Formula: 0.7K0.5Bi0.5TiO3:0.3ZnO
K0.5Bi0.5TiO3Powder calcination temperature is 850 DEG C, keeps the temperature 5h, and calcined temperature is 1020 DEG C, keeps the temperature 4h, K0.5Bi0.5TiO3: the sintering temperature of ZnO complex phase ceramic is 1050 DEG C, keeps the temperature 3h.The other the same as in Example 1.
Embodiment 5
Formula: 0.8K0.5Bi0.5TiO3:0.2ZnO
K0.5Bi0.5TiO3Powder calcination temperature is 800 DEG C, keeps the temperature 4h, and calcined temperature is 1000 DEG C, keeps the temperature 3h, K0.5Bi0.5TiO3: the sintering temperature of ZnO complex phase ceramic is 1020 DEG C, keeps the temperature 1.5h.The other the same as in Example 1.
Fine and close microstructure is presented in the ceramics sample prepared as shown in Figure 1, and defect is less.Also, ZnO's draws Enter to promote K0.5Bi0.5TiO3Particle increase.ZnO has sintering aids role, can be in K0.5Bi0.5TiO3Ceramic internal formation liquid phase, leads Its crystal grain is caused to grow up.
The K prepared as shown in Figure 20.5Bi0.5TiO3Powder is cubic perovskite structure (JCPDS36-0339) at room temperature, is added After entering ZnO, K0.5Bi0.5TiO3It is still tetragonal phase structure, but its tetragonality is obviously reduced.Observe 2 θ be 56 ° at (211)/ (112) after diffraction maximum is it can be found that be added ZnO, splitting degree is substantially reduced.Simultaneously it can also be observed that third phase Zn2TiO4 Phase (JCPDS 73-0578).
Pure K as shown in Figure 30.5Bi0.5TiO3It plants, in addition to maximum occurs in T=380 DEG C of temperature neighbouring real part of permittivity Outside, K0.5Bi0.5TiO3The imaginary part of dielectric constant of sample has a peak at 270 DEG C or so, shows near this temperature K0.5Bi0.5TiO3It is changed into relaxation ferroelectric, referred to as K by normal frroelectrics0.5Bi0.5TiO3Degenerate temperature.It is added 20% After nano-ZnO, abnormal phenomenon, explanation is nearby not observed at 270 DEG C in the spectrogram of dielectric real and imaginary parts K0.5Bi0.5TiO3Do not occur depolarization phenomenon in temperature ramp de, illustrates that the addition of ZnO inhibits K0.5Bi0.5TiO3's Degradation phenomena.

Claims (3)

1. a kind of K0.5Bi0.5TiO3: the unleaded compound ferroelectric ceramics of ZnO, by the K of perovskite structure0.5Bi0.5TiO3With nanoscale fibre The ZnO semiconductors coupling of zinc ore structure forms, and (1-x) K can be used in general formula0.5Bi0.5TiO3: xZnO indicates, wherein mole of ZnO Score x is 0.20~0.30.
2. unleaded compound ferroelectric ceramics as described in claim 1, it is characterized in that system is by having cubic perovskite structure K0.5Bi0.5TiO3The composite crystalline structure that principal crystalline phase is mutually constituted with wurtzite ZnO second.
3. unleaded compound ferroelectric ceramics as claimed in claim 2, it is characterized in that using the preparation process of two step solid phase methods, first Step has the K for stablizing perovskite structure for preparation0.5Bi0.5TiO3Ceramic powder, second step are to introduce nanoscale wurtzite structure ZnO, with K0.5Bi0.5TiO3Form composite ceramics.
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CN104788093A (en) * 2015-03-09 2015-07-22 南京大学 Preparation method for 0.94Bi0.5Na0.5TiO3-0.06BaTiO3 leadless piezoelectric ceramic

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