CN104402426B - A kind of bismuth ferrite-lead titanates-lead zinc niobate (BF-PT-PZN) ternary system high-temperature piezoelectric pottery - Google Patents
A kind of bismuth ferrite-lead titanates-lead zinc niobate (BF-PT-PZN) ternary system high-temperature piezoelectric pottery Download PDFInfo
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Abstract
The invention discloses a kind of novel bismuth ferrite lead titanates lead zinc niobate ternary system high-temperature piezoelectric pottery.In bismuth ferrite lead titanates (BF PT) system, it is firstly introduced ternary component lead zinc niobate (PZN), forms ternary solid solution system.It is effectively utilized the high-curie temperature characteristic that BF PT material has itself, and significantly improves the insulating properties of BF PT material by introducing ternary component PZN, make BF PT PZN material in the present invention be prone to polarized, thus obtain high piezoelectric constant.Novel tertiary high-curie temperature piezoelectric ceramic of the present invention has been prepared Curie temperature and has been up to 635oC, the 65 pC/N high-temperature piezoelectric potteries that piezoelectric constant reaches, ratio 2013, the high-temperature piezoelectric pottery that Xiaoli Tan is prepared in United States Patent (USP) possesses more excellent performance, and Curie temperature improves nearly 65oC and piezoelectric constant remain basically stable.The present invention makes the BF PT sill application in high-temperature piezoelectric field step forward a biggest step.
Description
Technical field
The present invention relates to novel tertiary system high-temperature piezoelectric ceramics, belong to high-temperature piezoelectric material field.
Background technology
Along with developing rapidly of modern science and technology, many electronic and electrical equipments are to selected piezoelectric device performance parameter
Have higher requirement.Wherein, the much industry such as Aero-Space, atomic energy, the energy, metallurgy, petrochemical industry and scientific research department
In the urgent need to the electronic equipment that can work at higher temperatures, these special dimension high-temperature piezoelectric material application
Become the task of top priority.High-temperature piezoelectric pottery requires that operating temperature is 300～800oC, the zirconium titanium that now commercialization degree is the highest
The Applicable temperature scope of lead plumbate (PZT) based piezoelectric ceramic materials is 300oBelow C, can not meet the application under hot conditions and wants
Ask.At present, the material supply section scholar of countries in the world is carrying out the grinding of piezoceramic material system of high-performance, high-curie temperature
Study carefully, try hard to develop high-curie temperature, piezoelectric property is excellent and temperature stability is good piezoceramic material.
Summary of the invention
It is an object of the invention to provide a kind of novel bismuth ferrite-lead titanates-lead zinc niobate ternary system high-temperature piezoelectric pottery.
A kind of novel bismuth ferrite of the present invention-lead titanates-lead zinc niobate (BF-PT-PZN) ternary system high-temperature piezoelectric pottery,
It is characterized in that there is following composition and mass fraction: (0.95-x) BF-xPT-0.05PZN, wherein 0.3 < x < 0.4.
The preparation method of the present invention a kind of novel B F-PT-PZN ternary system high-temperature piezoelectric pottery, it is characterised in that have
Following process and step:
First zinc niobate (ZnNb is synthesized2O6), with analytically pure ZnO and Nb2O5For raw material, mix according to mol ratio 1:1
After ball milling, 1250oCalcine 2 h under C and obtain the ZnNb of pure phase2O6；
B. synthesis BF-PT-PZN powder: with analytically pure Bi2O3、Fe2O3、PbO、TiO2ZnNb with synthesis2O6For former
Material, weigh 50g above-mentioned raw materials by above-mentioned composition and mass fraction and put in ball grinder, be subsequently adding 50 ml deionized waters and
1.5 ml ammoniacal liquor as the zirconium oxide bead that solvent and weight are raw material weight 0.8～1.5 times as ball-milling medium, rolling ball milling 24
h；After ball milling, ball milling slurry is poured in the china bowl of cleaning, insert 120oC constant temperature oven is dried, subsequently that powder is finely ground,
Put in crucible and calcine, synthesize BF-PT-PZN powder；Calcining curve is: from room temperature 5oC/min is warming up to 450oC, protects
Temperature 2 h, then 5oC/min is warming up to 800oC, is incubated 4 h, cools down with stove；After having calcined, powder will be synthesized finely ground, put into
In ball grinder, carry out second time ball milling；Afterwards, then carry out above-mentioned identical second time calcining and third time mechanical milling process；3rd
After the powder of discharging after secondary ball milling is dried, finely ground mistake 150 mesh sieve, obtain particle BF-PT-PZN synthetic powder tiny, uniform；
C. molding biscuit: dripping concentration in the synthetic powder prepared is 5% binding agent PVA, carries out granulation；Dripping quantity
For powder amount 7%；Dry-pressing formed under 150 MPa afterwards；Carry out binder removal after forming, finally obtain BF-PT-PZN element embryo；
Binder removal curve is: from room temperature 0.5oC/min is warming up to 450oC, is incubated 3 h, then 0.5oC/min is warming up to 600oC, protects
Temperature 3 h, cool down with stove；
D. pottery is sintered: above-mentioned gained BF-PT-PZN biscuit is placed on sealed sintering in crucible；Sintering curre is: from room
Temperature 5oC/min is warming up to 1020oC, is incubated 3 h, cools down with stove；
E. pottery Quenching Treatment: the ceramics sample sintered is put in crucible and seal, carry out later stage Quenching Treatment, quenching
Mechanism is 650oC is incubated 0.5 h, the most in deionized water chilling.
Feature for the present invention and mechanism
Bismuth ferrite-lead titanates (BF-PT) system solid solution Curie temperature at quasi-homotype phase boundary (MPB) place has exceeded 630oC.Additionally, BF-PT system solid solution also has the spontaneous strain of 18% at MPB, imply that this system exists superior piezoelectricity
Can, make BF-PT sill have broad application prospects in high-temperature piezoelectric field.But, due to binary BF-PT system material
Fe3+The leakage conductance that ion-labile valency forms Lacking oxygen and produces is serious, not only makes the measurement of its ferroelectric hysteresis loop become extremely difficult, very
To only obtaining Curie temperature accurately by Measuring Dielectric Constant.Great drawback in insulating properties limits BF-PT body
It is as high-temperature piezoelectric material application in practice.In order to strengthen the insulating properties of BF-PT system, reduce its coercive field intensity, enter
And obtaining the high-temperature piezoelectric material of excellent performance, people use multiple method to be modified it, and such as doping vario-property, technique changes
Enter and form ternary solid solution etc. with other materials.There are some researches show, BF-PT can be substantially improved by element doping
The inherent shortcoming of material, is improved its piezoelectric property, but is significantly dropped by the BF-PT piezoelectric Curie temperature of doping vario-property
Low.Finding in pursuing the research process of high-curie temperature and high tension performance, there is choice in both performance parameters each other.Cause
This, the relation between the two that is correctly balanced becomes the key of researching high-temperature piezoelectric ceramics.2013, Xiaoli Tan deliver
In one United States Patent (USP), introducing ternary component lead zirconates in BF-PT material, having obtained Curie temperature is 575oC, piezoelectricity
Constant (d33) be 64 pC/N high-temperature piezoelectric pottery.Its high Curie temperature makes this material have and is applied to high-temperature piezoelectric neck
The potentiality in territory, but its moderate piezoelectric constant need nonetheless remain for improving further.
The present invention, based on meeting the requirements at the higher level that piezoelectric is proposed by the device worked in high temperature environments, prepares
Curie temperature is high, the new type high temperature piezoelectric that piezoelectric constant is high.The invention provides a kind of novel tertiary high-curie temperature pressure
Electroceramics.In bismuth ferrite-lead titanates (BF-PT) system, it is firstly introduced ternary component lead zinc niobate (PZN), forms ternary solid
Solution system.Introducing on the premise of Curie temperature somewhat reduces on a small quantity of Relaxation Ferroelectrics lead zinc niobate, improves material
Insulating properties and piezoelectric property, and temperature stability also has significant improvement.Novel tertiary high-curie temperature of the present invention
Curie temperature T prepared by piezoelectric ceramicscUp to 635oC, depolarization temperature reaches 450oC, piezoelectric constant d3365 reached
The high-temperature piezoelectric pottery of pC/N, compares the high-temperature piezoelectric pottery that Xiaoli Tan in 2013 prepared in United States Patent (USP) and possesses more
Adding the performance of excellence, Curie temperature improves 60oC and piezoelectric constant d33Do not reduce.The present invention makes BF-PT sill exist
The application in high-temperature piezoelectric field has stepped forward a biggest step.
The BF-PT-PZN ternary ceramics that the present invention prepares has the feature of high-curie temperature and high tension performance, is full
Foot high-temperature piezoelectric application material requested provides new approaches.
Accompanying drawing explanation
Fig. 1 is X-ray diffraction (XRD) figure of BF-PT-PZN ceramics sample of the present invention.
Fig. 2 is the ferroelectric hysteresis loop figure of BF-PT-PZN ceramics sample of the present invention.
Fig. 3 is the high temperature dielectric properties figure of BF-PT-PZN ceramics sample of the present invention.
Fig. 4 is the high-temperature piezoelectric performance map of BF-PT-PZN ceramics sample of the present invention.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in detail.
Embodiment
Preparation process and step in the present embodiment are as described below.
Component is chosen: (1-x) BF-xPT-0.05PZN, x=0.35.Ternary component lead zinc niobate content is 5%.
First zinc niobate (ZnNb is synthesized2O6), with analytically pure ZnO and Nb2O5For raw material, mix according to mol ratio 1:1
After ball milling, 1250oCalcine 2 h under C and obtain the ZnNb of pure phase2O6。
B. synthesis BF-PT-PZN powder: with analytically pure Bi2O3、Fe2O3、PbO、TiO2ZnNb with synthesis2O6For former
Material, weighs above-mentioned raw materials by stoichiometric proportion needed for preparing 50 g 0.65BF-0.35PT-0.05PZN and puts in ball grinder, so
Rear addition 50 ml deionized water and 1.5 ml ammoniacal liquor are as the zirconium oxide bead work that solvent and weight are raw material weight 0.8～1.5 times
For ball-milling medium, rolling ball milling 24 h.After ball milling, ball milling slurry is poured in the china bowl of cleaning, insert 120oC constant temperature oven
Middle drying, subsequently that powder is finely ground, to put in crucible and calcine, synthesize BF-PT-PZN powder, calcining curve is: from room temperature 5oC/min is warming up to 450oC, is incubated 2 h, then 5oC/min is warming up to 800oC, is incubated 4 h, cools down with stove.Calcining completes
After, powder will be synthesized finely ground, put in ball grinder, carry out second time ball milling.Afterwards, then carry out above-mentioned identical second time calcining
With third time mechanical milling process.After after ball milling, the powder of discharging is dried for the third time, finely ground mistake 150 mesh sieve, obtain particle tiny, uniform
BF-PT-PZN synthetic powder.
C. molding biscuit: dripping concentration in the synthetic powder prepared is 5% binding agent PVA, carries out granulation.Dripping quantity
For powder amount 7%.Dry-pressing formed under 150 MPa afterwards.Carry out binder removal after forming, finally obtain BF-PT-PZN element embryo,
Binder removal curve is: from room temperature 0.5oC/min is warming up to 450oC, is incubated 3 h, then 0.5oC/min is warming up to 600oC, protects
Temperature 3 h, cool down with stove.
D. ceramic post sintering: above-mentioned gained BF-PT-PZN biscuit is placed on sealed sintering in crucible, and sintering curre is: from room
Temperature 5oC/min is warming up to 1020oC, is incubated 3 h, cools down with stove.
E. pottery Quenching Treatment: the ceramics sample sintered is put in crucible and seal, carry out later stage Quenching Treatment, quenching
Mechanism is 650oC is incubated 0.5 h, the most in deionized water chilling.Then the properties of sample is tested.
Gained BF-PT-PZN ternary ceramics of the present invention is characterized and performance test
1.X x ray diffractometer x (XRD) detects
Testing result is shown in X-ray diffraction (XRD) figure that Fig. 1, Fig. 1 are BF-PT-PZN of the present invention pottery.From Fig. 1 permissible
Find out that the perovskite structure that the phase structure of ceramics sample is tripartite's phase and Tetragonal coexists shows quasi-homotype phase boundary (MPB)
Feature.The phase structure of its quasi-homotype phase boundary imply that the piezoelectric property of its excellence.
2. ferroelectric properties test
Testing result is shown in the ferroelectric hysteresis loop figure that Fig. 2, Fig. 2 are BF-PT-PZN of the present invention pottery.Figure it is seen that it is ceramic
Sample reaches 180 kV/cm at extra electric field, under conditions of test frequency 10 Hz, still fails saturated.This explanation ceramics sample tool
There is the biggest coercive field intensity, it is difficult to polarization, may be relevant with the tetragonal distortion in crystal structure.Another angle, this Ceramic Like
Product can bear the biggest electric field, illustrates that ceramic structure is fine and close, and defect is less.
3. high temperature dielectric properties test
Testing result is shown in that Fig. 3, Fig. 3 are BF-PT-PZN of the present invention pottery high temperature dielectric properties figure under 1 MHz.From figure
It can be seen that ceramics sample dielectric constant is along with the rising of temperature, first increases and then decreases in 2, show obvious dielectric peak, be situated between
Electricity temperature corresponding to peak is exactly the Curie temperature T of samplec.It can be seen that the Curie temperature of this ternary ceramics sample
635oC.It should be noted that before dielectric peak, 500oThere is a dielectric " acromion " near C, the existence of " acromion " can
Can correspond near this temperature, there is tripartite and arrive the ferroelectric phase transition process of Tetragonal mutually.It addition, from the figure, it can be seen that sample
Dielectric loss value be slowly increased along with the rising of temperature, when temperature is increased to 500 from room temperatureoC, the increasing of dielectric loss value
Long very mild, illustrate that sample has fine temperature stability；When temperature continues to rise to 500oDuring about C, dielectric loss value
Steeply rise, when temperature reaches Curie temperature (635oC) time, dielectric loss value is also not above 1, illustrates that sample is at high temperature
Remain to keep high-insulativity, be conducive to its application in hot environment.And after exceeding Curie temperature when temperature, loss value by
Impact in high-temperature electrical conductivity is increased dramatically.
4. high-temperature piezoelectric performance test
Testing result is shown in the piezoelectric coefficient d that Fig. 4, Fig. 4 are BF-PT-PZN of the present invention pottery33And planar electromechanical coupling factor
KpVariation with temperature graph of a relation.Figure 4, it is seen that the piezoelectric coefficient d of ceramics sample33With planar electromechanical coupling factor Kp
In room temperature to 450oTemperature range kept stable between C, along with the rising of temperature slowly reduces；When temperature is increased to
450 oDuring C, piezoelectric coefficient d33With planar electromechanical coupling factor KpDecline rapidly.
The result of comprehensive above test analysis shows: the Curie temperature T of BF-PT-PZN ceramics sample of the present inventioncReach 635oC, its piezoelectric property compares binary BF-PT material has had significant raising, room temperature piezoelectric constant to reach 65 pC/N；And its pressure
Electrical property is less than 450 in temperatureoCan maintain a relatively stable state during C.
Claims (1)
1. a preparation method for bismuth ferrite-lead titanates-lead zinc niobate ternary system high-temperature piezoelectric pottery, this piezoelectric ceramics has
Following composition and mass fraction: (0.95-x) BF-xPT-0.05PZN, wherein 0.3 < x < 0.4；It is characterized in that having following
Process and step:
First zinc niobate (ZnNb is synthesized2O6), with analytically pure ZnO and Nb2O5For raw material, according to mol ratio 1:1 mixing and ball milling
After, 1250oCalcine 2 h under C and obtain the ZnNb of pure phase2O6；
B. synthesis BF-PT-PZN powder: with analytically pure Bi2O3、Fe2O3、PbO、TiO2ZnNb with synthesis2O6For raw material, by upper
State composition and mass fraction weighs 50 g above-mentioned raw materials and puts in ball grinder, be subsequently adding 50 ml deionized waters and 1.5 ml
Ammoniacal liquor as the zirconium oxide bead that solvent and weight are raw material weight 0.8～1.5 times as ball-milling medium, rolling ball milling 24 h；Ball
After mill, ball milling slurry is poured in the china bowl of cleaning, insert 120oC constant temperature oven is dried, subsequently that powder is finely ground, put into
Crucible is calcined, synthesizes BF-PT-PZN powder；Calcining curve is: from room temperature 5oC/min is warming up to 450oC, is incubated 2
H, then 5oC/min is warming up to 800oC, is incubated 4 h, cools down with stove；After having calcined, powder will be synthesized finely ground, put into ball milling
In tank, carry out second time ball milling；Afterwards, then carry out above-mentioned identical second time calcining and third time mechanical milling process；Ball for the third time
After the powder of discharging after mill is dried, finely ground mistake 150 mesh sieve, obtain particle BF-PT-PZN synthetic powder tiny, uniform；
C. molding biscuit: dripping concentration in the synthetic powder prepared is 5% binding agent PVA, carries out granulation；Dripping quantity is powder
The 7% of the scale of construction；Dry-pressing formed under 150 MPa afterwards；Carry out binder removal after forming, finally obtain BF-PT-PZN element embryo；Binder removal
Curve is: from room temperature 0.5oC/min is warming up to 450oC, is incubated 3 h, then 0.5oC/min is warming up to 600oC, is incubated 3
H, cools down with stove；
D. pottery is sintered: above-mentioned gained BF-PT-PZN biscuit is placed on sealed sintering in crucible；Sintering curre is: from room temperature 5oC/min is warming up to 1020oC, is incubated 3 h, cools down with stove；
E. pottery Quenching Treatment: put into by the ceramics sample sintered in crucible and seal, carries out later stage Quenching Treatment, quenching mechanism
It is 650oC is incubated 0.5 h, the most in deionized water chilling.
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| CN106810235A (en) * | 2017-01-23 | 2017-06-09 | 上海大学 | Bismuth ferrite lead titanates barium titanate ternary system high-temperature piezoelectric ceramics and preparation method thereof |
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| CN106007695B (en) * | 2016-04-26 | 2018-08-28 | 北京工业大学 | It is a kind of to utilize the disposable synthetic method of the compound multi-iron materials of presoma hydro-thermal process NFO-PZT-BFO |
| CN113248247A (en) * | 2021-06-23 | 2021-08-13 | 上海大学 | Ternary piezoelectric ceramic and preparation method and application thereof |
| CN118084473B (en) * | 2024-04-26 | 2024-07-23 | 同济大学 | Different-valence ion doped high-voltage electrical property lead-free bismuth ferrite-based piezoelectric ceramic material and preparation method thereof |
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| CN102603294A (en) * | 2012-03-23 | 2012-07-25 | 天津大学 | Method for preparing high-performance lanthanum-doped lead zinc niobate and lead zirconate titanate piezoelectric ceramic under condition with excessive lead |
| CN102633496A (en) * | 2012-04-09 | 2012-08-15 | 上海大学 | Method for preparing high-temperature and high-power piezoelectric transformers by using BLF-PTM (bismuth lanthanum ferrite-lead manganese titanate) piezoelectric ceramics |
| CN103951405A (en) * | 2014-04-09 | 2014-07-30 | 上海大学 | Ternary piezoceramic material with high Curie temperature and preparation method thereof |
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| JP5354538B2 (en) * | 2008-07-30 | 2013-11-27 | キヤノン株式会社 | Metal oxide and piezoelectric materials |
| TWI518048B (en) * | 2013-01-29 | 2016-01-21 | 佳能股份有限公司 | Piezoelectric material, piezoelectric device, and electronic apparatus |
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| CN102603294A (en) * | 2012-03-23 | 2012-07-25 | 天津大学 | Method for preparing high-performance lanthanum-doped lead zinc niobate and lead zirconate titanate piezoelectric ceramic under condition with excessive lead |
| CN102633496A (en) * | 2012-04-09 | 2012-08-15 | 上海大学 | Method for preparing high-temperature and high-power piezoelectric transformers by using BLF-PTM (bismuth lanthanum ferrite-lead manganese titanate) piezoelectric ceramics |
| CN103951405A (en) * | 2014-04-09 | 2014-07-30 | 上海大学 | Ternary piezoceramic material with high Curie temperature and preparation method thereof |
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| CN106810235A (en) * | 2017-01-23 | 2017-06-09 | 上海大学 | Bismuth ferrite lead titanates barium titanate ternary system high-temperature piezoelectric ceramics and preparation method thereof |
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