CN106810235A - Bismuth ferrite lead titanates barium titanate ternary system high-temperature piezoelectric ceramics and preparation method thereof - Google Patents
Bismuth ferrite lead titanates barium titanate ternary system high-temperature piezoelectric ceramics and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of bismuth ferrite lead titanates barium titanate ternary system high-temperature piezoelectric ceramics and preparation method thereof, BF PT BT high-temperature piezoelectrics ceramics are prepared for using solid reaction process, the insulating properties of BF PT materials are significantly improved by introducing ternary component BT in BF PT solid solution, there is piezoelectric constant very high simultaneously, reach 195 pC/N, and with Curie temperature high, 547 DEG C are reached, and its piezoelectric property can maintain a relatively stable state when temperature is less than 490 DEG C.Compared with commercial bismuth laminated piezoelectric, Curie temperature is approached, and piezoelectric modulus is its 5 times.
Description
Technical field
The present invention relates to a kind of piezoelectric and preparation method thereof, more particularly to a kind of multicomponent system high-temperature piezoelectric material
And preparation method thereof, it is applied to the functional material preparing technical field of sensor, driver and transducer.
Background technology
Piezoelectric ceramics is all widely used in numerous areas such as communication, household electrical appliances, aviation, detection and computers.With section
The fast development of technology, some special dimensions, such as aviation, automobile, petrochemical industry, active demand can be steady in high temperature environments
The fixed piezoelectric transducer for working, driver and transducer.
High-temperature piezoelectric material is the core sensing element of high temperature piezoelectric device.But function admirable, Curie temperature pressure high
Electroceramics material is with present case or fewer.This is allowed for for a long time, and Special high-temperature piezoelectric device has to use
The monocrystalline piezoelectric material of complex manufacturing, high cost.Therefore, high-curie temperature piezoelectric ceramic material of the exploitation with excellent properties
Material has turned into the task of top priority.At present, scientist does to find the piezoelectric ceramics that can be suitably used under hot environment all over the world
Go out unremitting effort.
The BF-PT solid solution of bismuth ferrite-lead titanates is a kind of piezoelectric with quasi- homotype phase boundary and high-Curie-point,
High temperature piezoelectric device field has broad application prospects.But, BF-PT ceramics coercive fields are powerful, it is difficult to polarize, dielectric loss
Greatly, mechanical quality factor is low, limits its application in high temperature piezoelectric device.In order to strengthen insulating properties, the drop of BF-PT ceramics
Low its coercive field intensity, and then the high-temperature piezoelectric material of excellent performance is obtained, people are modified using various methods to it, for example
Doping vario-property, process modification and form ternary solid solution etc. with other materials.There are some researches show by element doping energy
The inherent shortcoming of BF-PT materials is enough substantially improved, its piezoelectric property is improved, but the BF-PT piezoelectrics for passing through doping vario-property
Curie temperature is substantially reduced.Found in the research process of high-curie temperature and high tension performance is pursued, both performance parameters
Exist each other and accept or reject, which has limited the application field of BF-PT piezoelectrics.
The content of the invention
In order to solve prior art problem, it is an object of the invention to overcome the shortcomings of that prior art is present, there is provided a kind of
Bismuth ferrite-lead titanates-barium titanate ternary system high-temperature piezoelectric ceramics and preparation method thereof, balance Curie temperature and piezoelectric property two
Relation between person, develops new high-temperature piezoelectric ceramics.The present invention leads to the titanium that introducing ternary has perovskite structure excessively
Sour barium has prepared that Curie temperature is high, piezoelectric constant new type high temperature piezoelectric high, bismuth ferrite-lead titanates-metatitanic acid of the present invention
Barium ternary system high-temperature piezoelectric ceramics meet the requirements at the higher level that the device for working in high temperature environments is proposed to piezoelectric, with
Commercial bismuth laminated piezoelectric is compared, and Curie temperature and piezoelectric modulus are with the obvious advantage, with significant application prospect.
Purpose is created to reach foregoing invention, the present invention uses following technical proposals：
A kind of bismuth ferrite-lead titanates-barium titanate ternary system high-temperature piezoelectric ceramics, with following composition and quality mole
Fraction：
Bismuth ferrite in (1-x) BF-xPT-0.15BT, i.e. BF-PT-BT ternary systems：Lead titanates：The mole of barium titanate
The ratio between be (1-x)：x：0.15, and 0.19≤x≤0.27.
Used as currently preferred technical scheme, chemical formula meets following number range：X=1:(0.19~0.23).
A kind of preparation method of bismuth ferrite-lead titanates-barium titanate ternary system high-temperature piezoelectric ceramics, comprises the following steps：
A. BF-PT-BT powders are synthesized：
With pure Bi2O3、Fe2O3、PbO、TiO2、BaCO3And MnO2It is raw material, is (1-x) BF-xPT- by chemical formula is prepared
Stoichiometric proportion needed for the BF-PT-BT ternary systems of 0.15BT weighs above-mentioned raw materials, i.e., in control BF-PT-BT ternary systems
Bismuth ferrite：Lead titanates：The ratio between mole of barium titanate is (1-x)：x：0.15；And reducing material proportioning will also meet following chemistry
Number range in formula is x=(0.19~0.23)；Above-mentioned raw materials after weighing are mixed, by grinding at least one times
Mill, screening and high-temperature calcination technique obtain that particle is tiny and uniform BF-PT-BT synthetic powders；As currently preferred skill
Art scheme is as follows by grinding at least one times, screening and high-temperature calcination technique：According to the ball-milling technology ratio of following pellet water
Example carries out first time ball milling：
Above-mentioned raw materials after weighing are amounted into 30g to be put into ball grinder, it is 45g to be subsequently adding 30ml deionized waters and weight
The zirconia ball of different-diameter size and shape carries out first time ball milling at least 24h；
Then first time sieving treatment will be carried out by the slurry obtained after first time ball milling, zirconium oxide is leached by screen cloth
Bead, then slurry is poured into ceramic bowl, the rim of a bowl covering aluminium foil dries at least 120 DEG C in the baking oven being put into slurry
It is dry to obtain dry powder, after then powder crosses at least mesh screen of 120 mesh, then the powder after sieving is put into crucible carries out
High-temperature calcination synthesizes BF-PT-PT powders, and first time high-temperature calcination process curve is：
The first stage of calcining is to be warming up to 450 DEG C according to the programming rate of at least 5 DEG C/min since room temperature, and insulation is extremely
Few 2h, then the second stage calcined, the second stage of calcining are warming up to 750- according to the programming rate of at least 5 DEG C/min
850 DEG C, then at least 4h is incubated, after the second stage for completing calcining, furnace cooling completes first time high-temperature burning process；
After the completion of first time high-temperature calcination, the synthesis powder obtained after first time high-temperature calcination is carried out into finely ground place again
Reason, is put into ball grinder, carries out second ball milling, and second ball-milling technology is identical with first time ball-milling technology, by second
After secondary ball milling, the slurry that will be obtained after ball milling carries out second sieving treatment, second sieve handling process and first time mistake
Sieve handling process is identical, then carry out with second high-temperature calcination of identical of first time high-temperature calcination technique, then carry out again and the
Ball-milling technology identical third time mechanical milling process, discharge drying after third time ball milling, then crosses at least 120 mesh sieves, obtains
To particle is tiny and uniform BF-PT-BT synthetic powders；As currently preferred technical scheme, it is being by preparing chemical formula
When stoichiometric proportion needed for the BF-PT-BT ternary systems of (1-x) BF-xPT-0.15BT weighs raw material, also meet according to chemical formula
Following numerical relation：X=1：(0.19~0.23).To control lead titanates to remove consumption.
B. molding biscuit：
The binding agent that mass concentration is not less than 5% is added dropwise in the BF-PT-BT synthetic powders prepared in the step a
PVA, is granulated, and binding agent PVA dripping quantities are at least the 7% of BF-PT-BT synthetic powder quality, afterwards will under 100MPa
The compound of BF-PT-BT synthetic powders and binding agent PVA tentatively carries out pressure forming for minimum diameter is 12mm and minimum thickness
It is the disk blank of 1mm, then proceeds to few 200MPa isostatic pressings for first base, after isostatic pressed, dumping is carried out to first base,
BF-PT-BT element embryos are finally obtained, binder removal curve is：
First stage since room temperature, at least 3h is incubated after 720min is warming up to 450 DEG C, then by 300min
3h is at least incubated after being warming up to 600 DEG C, then furnace cooling, that is, completes binder removal process, obtain BF-PT-BT precast body bases
Material；
C. ceramics are sintered：
Sealed sintering during the BF-PT-BT precast body blanks prepared in the step b are placed on into crucible, sintering curre is：
1100-1200 DEG C is warming up to the programming rate of 5 DEG C/min since room temperature, at least 2h, then furnace cooling is then incubated, finally
BF-PT-BT ternary system high-temperature piezoelectric ceramic products are obtained.
The present invention compared with prior art, substantive distinguishing features and remarkable advantage is obviously protruded with following：
1. the characteristics of BF-PT-BT ternary ceramics of the present invention have high-curie temperature and high tension performance, by introducing the 3rd
First component BT significantly improves the insulating properties of BF-PT materials, remains to keep high-insulativity at high temperature, is conducive to it in high temperature
Application in environment；
2. BF-PT-BT ternary ceramics of the present invention have piezoelectric constant and Curie's temperature high very high in BF-PT solid solution
Spend, and its piezoelectric property can maintain a relatively stable state in high temperature, with commercial bismuth laminated piezoelectric phase
Than Curie temperature is approached, and piezoelectric modulus is with the obvious advantage.
Brief description of the drawings
Fig. 1 is X-ray diffraction (XRD) figure of the BF-PT-BT ceramics samples of the embodiment of the present invention one.
Fig. 2 is the ferroelectric hysteresis loop figure of the BF-PT-BT ceramics samples of the embodiment of the present invention one.
Fig. 3 is the high temperature dielectric properties figure of the BF-PT-BT ceramics samples of the embodiment of the present invention one.
Fig. 4 is the high-temperature piezoelectric performance map of the BF-PT-BT ceramics samples of the embodiment of the present invention one.
Fig. 5 is X-ray diffraction (XRD) figure of the BF-PT-BT ceramics samples of the embodiment of the present invention two.
Fig. 6 is the ferroelectric hysteresis loop figure of the BF-PT-BT ceramics samples of the embodiment of the present invention two.
Fig. 7 is the high temperature dielectric properties figure of the BF-PT-BT ceramics samples of the embodiment of the present invention two.
Fig. 8 is the high-temperature piezoelectric performance map of the BF-PT-BT ceramics samples of the embodiment of the present invention two.
Fig. 9 is X-ray diffraction (XRD) figure of the BF-PT-BT ceramics samples of the embodiment of the present invention three.
Figure 10 is the ferroelectric hysteresis loop figure of the BF-PT-BT ceramics samples of the embodiment of the present invention three.
Figure 11 is the high temperature dielectric properties figure of the BF-PT-BT ceramics samples of the embodiment of the present invention three.
Figure 12 is the high-temperature piezoelectric performance map of the BF-PT-BT ceramics samples of the embodiment of the present invention three.
Specific embodiment
Details are as follows for the preferred embodiments of the present invention：
Embodiment one：
In the present embodiment, a kind of bismuth ferrite-lead titanates-barium titanate ternary system high-temperature piezoelectric ceramics, with following
Composition and quality molar fraction：Bismuth ferrite in 0.62BF-0.23PT-0.15BT, i.e. BF-PT-BT ternary systems：Lead titanates：
The ratio between mole of barium titanate is 0.62：0.23：0.15.The present embodiment component is chosen and uses (1-x) BF-xPT-0.15BT, x=
0.23, ternary component barium titanate content is 15%.
The preparation method of the present embodiment bismuth ferrite-lead titanates-barium titanate ternary system high-temperature piezoelectric ceramics, including following step
Suddenly：
A. BF-PT-BT powders are synthesized：
With pure Bi2O3、Fe2O3、PbO、TiO2、BaCO3And MnO2It is raw material, is 0.62BF- by chemical formula is prepared
Stoichiometric proportion needed for the BF-PT-BT ternary systems of 0.23PT-0.15BT weighs above-mentioned raw materials, that is, control BF-PT-BT ternarys
Bismuth ferrite in system：Lead titanates：The ratio between mole of barium titanate is 0.62：0.23：0.15；Above-mentioned raw materials after weighing are entered
Row mixing, obtains that particle is tiny and uniform BF-PT-BT synthetic powders by multiple grinding, screening and high-temperature calcination technique,
It is specific as follows：
The ball-milling technology ratio for being first according to following pellet water carries out first time ball milling：
Above-mentioned raw materials after weighing are amounted into 30g to be put into ball grinder, it is 45g to be subsequently adding 30ml deionized waters and weight
The zirconia ball of different-diameter size and shape carries out first time ball milling 24h；
Then first time sieving treatment will be carried out by the slurry obtained after first time ball milling, zirconium oxide is leached by screen cloth
Bead, then slurry is poured into ceramic bowl, the rim of a bowl covering aluminium foil carries out to slurry at 120 DEG C drying in the baking oven being put into
To dry powder, after then powder crosses the mesh screen of 120 mesh, then the powder after sieving is put into crucible carries out first time high temperature
Calcining synthesizes BF-PT-PT powders, and first time high-temperature calcination process curve is：
The first stage of calcining is to be warming up to 450 DEG C according to the programming rate of 5 DEG C/min since room temperature, is incubated 2h, then
The second stage calcined, the second stage of calcining is warming up to 750 DEG C according to the programming rate of 5 DEG C/min, then is incubated 4h,
After completing the second stage of calcining, furnace cooling completes first time high-temperature burning process；
After the completion of first time high-temperature calcination, the synthesis powder obtained after first time high-temperature calcination is carried out into finely ground place again
Reason, is put into ball grinder, carries out second ball milling, and second ball-milling technology is identical with first time ball-milling technology, by second
After secondary ball milling, the slurry that will be obtained after ball milling carries out second sieving treatment, second sieve handling process and first time mistake
Sieve handling process is identical, then carry out with second high-temperature calcination of identical of first time high-temperature calcination technique, then carry out again and the
Ball-milling technology identical third time mechanical milling process, discharge drying after third time ball milling, then crosses 120 mesh sieves, obtains
Grain is tiny and uniform BF-PT-BT synthetic powders；
B. molding biscuit：
The binding agent PVA that mass concentration is 5% is added dropwise in the BF-PT-BT synthetic powders prepared in the step a,
Granulated, binding agent PVA dripping quantities are the 7% of BF-PT-BT synthetic powder quality, afterwards by BF-PT-BT under 100MPa
The compound of synthetic powder and binding agent PVA tentatively carry out pressure forming be a diameter of 12mm and thickness for 1mm disk blank,
200MPa isostatic pressings are then carried out for first base, after isostatic pressed, dumping is carried out to first base, finally obtain BF-PT-BT elements
Embryo, binder removal curve is：
First stage since room temperature, carries out insulation 3h, then heat up by 300min after 720min is warming up to 450 DEG C
3h is incubated after to 600 DEG C, then furnace cooling completes binder removal process, obtains BF-PT-BT precast body blanks；
C. ceramics are sintered：
Sealed sintering during the BF-PT-BT precast body blanks prepared in the step b are placed on into crucible, sintering curre is：
1120 DEG C are warming up to the programming rate of 5 DEG C/min since room temperature, 2h, then furnace cooling is then incubated, BF- is finally obtained
PT-BT ternary system high-temperature piezoelectric ceramic products.
The present embodiment gained BF-PT-BT ternary ceramics are characterized and performance test
1.X x ray diffractometer xs (XRD) are detected
X-ray diffractometer (XRD) detection is carried out to the present embodiment gained BF-PT-BT ternary ceramics, testing result is shown in Fig. 1,
Fig. 1 is X-ray diffraction (XRD) figure of BF-PT-BT ceramics of the present invention.From figure 1 it appears that the phase structure of ceramics sample
It is the perovskite structure that tripartite's phase and Tetragonal coexist, shows quasi- homotype phase boundary (MPB) feature.The thing phase of its quasi- homotype phase boundary
Structure imply that its excellent piezoelectric property.
2. ferroelectric properties test
The present embodiment gained BF-PT-BT ternary ceramics are carried out with ferroelectric properties test, testing result is shown in that Fig. 2, Fig. 2 are this
Ferroelectric hysteresis loop figure (test frequency 10Hz) of invention BF-PT-BT ceramics.Figure it is seen that ceramics sample can withstand up to
The electric field of 70kV/cm, residual polarization value and coercive field are respectively 15 μ C/cm2And 30kV/cm.
3. high temperature dielectric properties test
High temperature dielectric properties test is carried out to the present embodiment gained BF-PT-BT ternary ceramics, testing result is shown in Fig. 3, Fig. 3
It is high temperature dielectric properties figure of the BF-PT-BT of the present invention ceramics under 1MHz.From figure 3, it can be seen that ceramics sample dielectric constant
As the rising of temperature, first increases and then decreases show obvious dielectric peak, the temperature corresponding to dielectric peak is exactly the residence of sample
In temperature Tc.From figure 3, it can be seen that the Curie temperature of this ternary ceramics sample is at 547 DEG C.In addition, from the figure, it can be seen that
The dielectric loss value of sample is slowly increased with the rising of temperature, when temperature is increased to 547 DEG C from room temperature, dielectric loss value
Increase very gentle, illustrate that sample has fine temperature stability；When temperature reaches 547 DEG C of Curie temperature, dielectric loss refers to
Less than 0.25, illustrate that sample remains to keep high-insulativity at high temperature, be conducive to its application in hot environment.
4. high-temperature piezoelectric performance test
High-temperature piezoelectric performance test is carried out to the present embodiment gained BF-PT-BT ternary ceramics, testing result is shown in Fig. 4, Fig. 4
It is BF-PT-BT ceramic flat surfaces electromechanical coupling factor k of the present inventionpVariation with temperature graph of a relation.Figure 4, it is seen that ceramic
Sample plane electromechanical coupling factor kpIn room temperature to the temperature range kept stable between 490 DEG C, with the rising of temperature
It is slow to raise；When temperature is increased to 490 DEG C, planar electromechanical coupling factor kpIt is rapid to decline.
Embodiment two：
The present embodiment is essentially identical with embodiment one, is particular in that：
In the present embodiment, a kind of bismuth ferrite-lead titanates-barium titanate ternary system high-temperature piezoelectric ceramics, with following
Composition and quality molar fraction：Bismuth ferrite in 0.66BF-0.19PT-0.15BT, i.e. BF-PT-BT ternary systems：Lead titanates：
The ratio between mole of barium titanate is 0.66：0.19：0.15.The present embodiment component is chosen and uses (1-x) BF-xPT-0.15BT, x=
0.19, ternary component barium titanate content is 15%.
The preparation method of the present embodiment bismuth ferrite-lead titanates-barium titanate ternary system high-temperature piezoelectric ceramics, including following step
Suddenly：
A. BF-PT-BT powders are synthesized：
With pure Bi2O3、Fe2O3、PbO、TiO2、BaCO3And MnO2It is raw material, is 0.66BF- by chemical formula is prepared
Stoichiometric proportion needed for the BF-PT-BT ternary systems of 0.19PT-0.15BT weighs above-mentioned raw materials, that is, control BF-PT-BT ternarys
Bismuth ferrite in system：Lead titanates：The ratio between mole of barium titanate is 0.66：0.19：0.15；Above-mentioned raw materials after weighing are entered
Row mixing, obtains that particle is tiny and uniform BF-PT-BT synthetic powders by multiple grinding, screening and high-temperature calcination technique,
It is specific as follows：
The ball-milling technology ratio for being first according to following pellet water carries out first time ball milling：
Above-mentioned raw materials after weighing are amounted into 30g to be put into ball grinder, it is 45g to be subsequently adding 30ml deionized waters and weight
The zirconia ball of different-diameter size and shape carries out first time ball milling 24h；Then by by obtaining after first time ball milling
Slurry carries out first time sieving treatment, and zirconia ball is leached by screen cloth, then slurry is poured into ceramic bowl, the rim of a bowl aluminium coating
Paper tinsel, to slurry dry obtaining dry powder at 120 DEG C in the baking oven being put into, after then powder crosses the mesh screen of 120 mesh,
The powder after sieving is put into crucible again carry out first time high-temperature calcination synthesis BF-PT-PT powders, first time high-temperature calcination work
Skill curve is：
The first stage of calcining is to be warming up to 450 DEG C according to the programming rate of 5 DEG C/min since room temperature, is incubated 2h, then
The second stage calcined, the second stage of calcining is warming up to 850 DEG C according to the programming rate of 5 DEG C/min, then is incubated 4h,
After completing the second stage of calcining, furnace cooling completes first time high-temperature burning process；
After the completion of first time high-temperature calcination, the synthesis powder obtained after first time high-temperature calcination is carried out into finely ground place again
Reason, is put into ball grinder, carries out second ball milling, and second ball-milling technology is identical with first time ball-milling technology, by second
After secondary ball milling, the slurry that will be obtained after ball milling carries out second sieving treatment, second sieve handling process and first time mistake
Sieve handling process is identical, then carry out with second high-temperature calcination of identical of first time high-temperature calcination technique, then carry out again and the
Ball-milling technology identical third time mechanical milling process, discharge drying after third time ball milling, then crosses 120 mesh sieves, obtains
Grain is tiny and uniform BF-PT-BT synthetic powders；
B. molding biscuit：
The binding agent PVA that mass concentration is 5% is added dropwise in the BF-PT-BT synthetic powders prepared in the step a,
Granulated, binding agent PVA dripping quantities are the 7% of BF-PT-BT synthetic powder quality, afterwards by BF-PT-BT under 100MPa
The compound of synthetic powder and binding agent PVA tentatively carry out pressure forming be a diameter of 12mm and thickness for 1mm disk blank,
200MPa isostatic pressings are then carried out for first base, after isostatic pressed, dumping is carried out to first base, finally obtain BF-PT-BT elements
Embryo, binder removal curve is：
First stage since room temperature, carries out insulation 3h, then heat up by 300min after 720min is warming up to 450 DEG C
3h is incubated after to 600 DEG C, then furnace cooling completes binder removal process, obtains BF-PT-BT precast body blanks；
C. ceramics are sintered：
Sealed sintering during the BF-PT-BT precast body blanks prepared in the step b are placed on into crucible, sintering curre is：
1100 DEG C are warming up to the programming rate of 5 DEG C/min since room temperature, 2h, then furnace cooling is then incubated, BF- is finally obtained
PT-BT ternary system high-temperature piezoelectric ceramic products.
The present embodiment gained BF-PT-BT ternary ceramics are characterized and performance test
1.X x ray diffractometer xs (XRD) are detected
X-ray diffractometer (XRD) detection is carried out to the present embodiment gained BF-PT-BT ternary ceramics, testing result is shown in Fig. 5,
Fig. 5 is X-ray diffraction (XRD) figure of BF-PT-BT ceramics of the present invention.From figure 5 it can be seen that the phase structure of ceramics sample
It is the perovskite structure of tripartite's phase.
2. ferroelectric properties test
The present embodiment gained BF-PT-BT ternary ceramics are carried out with ferroelectric properties test, testing result is shown in that Fig. 6, Fig. 6 are this
Ferroelectric hysteresis loop figure (test frequency 10Hz) of invention BF-PT-BT ceramics.From fig. 6, it can be seen that ceramics sample can withstand up to
The electric field of 75kV/cm, residual polarization value and coercive field are respectively 20 μ C/cm2And 30kV/cm.
3. high temperature dielectric properties test
High temperature dielectric properties test is carried out to the present embodiment gained BF-PT-BT ternary ceramics, testing result is shown in Fig. 7, Fig. 7
It is high temperature dielectric properties figure of the BF-PT-BT of the present invention ceramics under 1MHz.It can be seen from figure 7 that ceramics sample dielectric constant
As the rising of temperature, first increases and then decreases show obvious dielectric peak, the temperature corresponding to dielectric peak is exactly the residence of sample
In temperature Tc.The Curie temperature of ternary ceramics sample manufactured in the present embodiment is at 585 DEG C.In addition, be can see from test result,
The dielectric loss value of sample is slowly increased with the rising of temperature, when temperature is increased to 585 DEG C from room temperature, dielectric loss value
Increase very gentle, illustrate that sample has fine temperature stability；When temperature reaches 585 DEG C of Curie temperature, dielectric loss refers to
Less than 0.25, illustrate that sample remains to keep high-insulativity at high temperature, be conducive to its application in hot environment.
4. high-temperature piezoelectric performance test
High-temperature piezoelectric performance test is carried out to the present embodiment gained BF-PT-BT ternary ceramics, testing result is shown in Fig. 8, Fig. 8
It is BF-PT-BT ceramic flat surfaces electromechanical coupling factor k of the present inventionpVariation with temperature graph of a relation.As can be seen from Figure 8, ceramics
Sample plane electromechanical coupling factor kpIn room temperature to the temperature range kept stable between 480 DEG C, with the rising of temperature
It is slow to raise；When temperature is increased to 480 DEG C, planar electromechanical coupling factor kpIt is rapid to decline.
The present embodiment significantly improves the insulation of BF-PT materials in BF-PT solid solution by introducing ternary component BT
Performance, while having piezoelectric constant very high, reaches 125pC/N, and with Curie temperature high, reaches 585 DEG C, and it is pressed
Electrical property can maintain a relatively stable state when temperature is less than 585 DEG C.Compared with commercial bismuth laminated piezoelectric,
Curie temperature is approached, and piezoelectric modulus reaches its 3 times or so.
Embodiment three：
The present embodiment is substantially the same as in the previous example, and is particular in that：
In the present embodiment, a kind of bismuth ferrite-lead titanates-barium titanate ternary system high-temperature piezoelectric ceramics, with following
Composition and quality molar fraction：Bismuth ferrite in 0.58BF-0.27PT-0.15BT, i.e. BF-PT-BT ternary systems：Lead titanates：
The ratio between mole of barium titanate is 0.58：0.27：0.15.The present embodiment component is chosen and uses (1-x) BF-xPT-0.15BT, x=
0.27, ternary component barium titanate content is 15%.
The preparation method of the present embodiment bismuth ferrite-lead titanates-barium titanate ternary system high-temperature piezoelectric ceramics, including following step
Suddenly：
A. BF-PT-BT powders are synthesized：
With pure Bi2O3、Fe2O3、PbO、TiO2、BaCO3And MnO2It is raw material, by preparing chemical formula 0.58BF-0.27PT-
Stoichiometric proportion needed for the BF-PT-BT ternary systems of 0.15BT weighs above-mentioned raw materials, i.e., in control BF-PT-BT ternary systems
Bismuth ferrite：Lead titanates：The ratio between mole of barium titanate is 0.58：0.27：0.15；Above-mentioned raw materials after weighing are mixed,
Obtain that particle is tiny and uniform BF-PT-BT synthetic powders by multiple grinding, screening and high-temperature calcination technique, specifically such as
Under
The ball-milling technology ratio for being first according to following pellet water carries out first time ball milling：
Above-mentioned raw materials after weighing are amounted into 30g to be put into ball grinder, it is 45g to be subsequently adding 30ml deionized waters and weight
The zirconia ball of different-diameter size and shape carries out first time ball milling 24h；
Then first time sieving treatment will be carried out by the slurry obtained after first time ball milling, zirconium oxide is leached by screen cloth
Bead, then slurry is poured into ceramic bowl, the rim of a bowl covering aluminium foil carries out to slurry at 120 DEG C drying in the baking oven being put into
To dry powder, after then powder crosses the mesh screen of 120 mesh, then the powder after sieving is put into crucible carries out first time high temperature
Calcining synthesizes BF-PT-PT powders, and first time high-temperature calcination process curve is：
The first stage of calcining is to be warming up to 450 DEG C according to the programming rate of 5 DEG C/min since room temperature, is incubated 2h, then
The second stage calcined, the second stage of calcining is warming up to 850 DEG C according to the programming rate of 5 DEG C/min, then is incubated 4h,
After completing the second stage of calcining, furnace cooling completes first time high-temperature burning process；
After the completion of first time high-temperature calcination, the synthesis powder obtained after first time high-temperature calcination is carried out into finely ground place again
Reason, is put into ball grinder, carries out second ball milling, and second ball-milling technology is identical with first time ball-milling technology, by second
After secondary ball milling, the slurry that will be obtained after ball milling carries out second sieving treatment, second sieve handling process and first time mistake
Sieve handling process is identical, then carry out with second high-temperature calcination of identical of first time high-temperature calcination technique, then carry out again and the
Ball-milling technology identical third time mechanical milling process, discharge drying after third time ball milling, then crosses 120 mesh sieves, obtains
Grain is tiny and uniform BF-PT-BT synthetic powders；
B. molding biscuit：
The binding agent PVA that mass concentration is 5% is added dropwise in the BF-PT-BT synthetic powders prepared in the step a,
Granulated, binding agent PVA dripping quantities are the 7% of BF-PT-BT synthetic powder quality, afterwards by BF-PT-BT under 100MPa
The compound of synthetic powder and binding agent PVA tentatively carry out pressure forming be a diameter of 12mm and thickness for 1mm disk blank,
200MPa isostatic pressings are then carried out for first base, after isostatic pressed, dumping is carried out to first base, finally obtain BF-PT-BT elements
Embryo, binder removal curve is：
First stage since room temperature, carries out insulation 3h, then heat up by 300min after 720min is warming up to 450 DEG C
3h is incubated after to 600 DEG C, then furnace cooling completes binder removal process, obtains BF-PT-BT precast body blanks；
C. ceramics are sintered：
Sealed sintering during the BF-PT-BT precast body blanks prepared in the step b are placed on into crucible, sintering curre is：
1200 DEG C are warming up to the programming rate of 5 DEG C/min since room temperature, 2h, then furnace cooling is then incubated, BF- is finally obtained
PT-BT ternary system high-temperature piezoelectric ceramic products.
The present embodiment gained BF-PT-BT ternary ceramics are characterized and performance test
1.X x ray diffractometer xs (XRD) are detected
X-ray diffractometer (XRD) detection is carried out to the present embodiment gained BF-PT-BT ternary ceramics, testing result is shown in Fig. 9,
Fig. 9 is X-ray diffraction (XRD) figure of BF-PT-BT ceramics of the present invention.It can be seen in figure 9 that, the phase structure of ceramics sample
It is Tetragonal perovskite structure.
2. ferroelectric properties test
Ferroelectric properties test is carried out to the present embodiment gained BF-PT-BT ternary ceramics, testing result is shown in Figure 10, Tu10Wei
Ferroelectric hysteresis loop figure (test frequency 10Hz) of BF-PT-BT ceramics of the present invention.From fig. 10 it can be seen that ceramics sample can bear
The up to electric field of 70kV/cm, residual polarization value and coercive field are respectively 15 μ C/cm2And 35kV/cm.
3. high temperature dielectric properties test
High temperature dielectric properties test is carried out to the present embodiment gained BF-PT-BT ternary ceramics, testing result is shown in Figure 11, figure
11 is high temperature dielectric properties figure of the BF-PT-BT of the present invention ceramics under 1MHz.It can be seen from fig. 11 that ceramics sample dielectric
Constant shows obvious dielectric peak with the rising of temperature, first increases and then decreases, and the temperature corresponding to dielectric peak is exactly sample
Curie temperature Tc.The Curie temperature of ternary ceramics sample manufactured in the present embodiment is at 505 DEG C.In addition, can be with from test result
See, the dielectric loss value of sample is slowly increased with the rising of temperature, when temperature is increased to 505 DEG C from room temperature, dielectric is damaged
The growth of consumption value is very gentle, illustrates that sample has fine temperature stability；When temperature reaches 505 DEG C of Curie temperature, dielectric
It is lost and refers to less than 0.3, illustrate that sample remains to keep high-insulativity at high temperature, is conducive to its application in hot environment.
4. high-temperature piezoelectric performance test
High-temperature piezoelectric performance test is carried out to the present embodiment gained BF-PT-BT ternary ceramics, testing result is shown in Figure 12, figure
12 is BF-PT-BT ceramic flat surfaces electromechanical coupling factor k of the present inventionpVariation with temperature graph of a relation.In figure 12 it can be seen that
Ceramics sample planar electromechanical coupling factor kpIn room temperature to the temperature range kept stable between 440 DEG C, with temperature
Raise slow rising；When temperature is increased to 440 DEG C, planar electromechanical coupling factor kpIt is rapid to decline.
The result of the test analysis of BF-PT-BT ternary ceramics samples prepared by comprehensive above example of the present invention shows：
The Curie temperature T of BF-PT-BT ternary ceramics samples prepared by above example of the present inventionc505 DEG C are reached, its pressure
Electrical property has significant raising compared to binary BF-PT materials, and room temperature piezoelectric constant reaches 195pC/N；And its piezoelectric property
Can be maintained a relatively stable state when temperature is less than 490 DEG C.BF-PT-BT ternarys pottery prepared by above example of the present invention
The characteristics of porcelain has high-curie temperature and high tension performance, is significantly carried in BF-PT solid solution by introducing ternary component BT
The insulating properties of BF-PT materials high, while there is piezoelectric constant and Curie temperature high very high, and its piezoelectric property exists
Temperature can maintain a relatively stable state when being less than 490 DEG C.Compared with commercial bismuth laminated piezoelectric, Curie temperature
Close, piezoelectric modulus can reach its more than 5 times.
The embodiment of the present invention is illustrated above in conjunction with accompanying drawing, but the invention is not restricted to above-described embodiment, can be with
The purpose of innovation and creation of the invention makes various changes, under all Spirit Essence and principle according to technical solution of the present invention
Change, modification, replacement, the combination or simplified made, should be equivalent substitute mode, as long as meeting goal of the invention of the invention,
Technology without departing from bismuth ferrite-lead titanates of the present invention-barium titanate ternary system high-temperature piezoelectric ceramics and preparation method thereof is former
Reason and inventive concept, belong to protection scope of the present invention.
Claims (5)
1. a kind of bismuth ferrite-lead titanates-barium titanate ternary system high-temperature piezoelectric is ceramic, it is characterised in that：With following composition
And quality molar fraction：
Bismuth ferrite in (1-x) BF-xPT-0.15BT, i.e. BF-PT-BT ternary systems：Lead titanates：The ratio between mole of barium titanate
It is (1-x)：x:0.15, and 0.19≤x≤0.23.
2. bismuth ferrite-lead titanates-barium titanate ternary system high-temperature piezoelectric is ceramic according to claim 1, it is characterised in that change
Formula also meets following numerical relation：X=1:(0.19~0.23).
3. the preparation method of a kind of bismuth ferrite-lead titanates-barium titanate ternary system high-temperature piezoelectric ceramics, it is characterised in that including
Following steps：
A. BF-PT-BT powders are synthesized：
With pure Bi2O3、Fe2O3、PbO、TiO2、BaCO3And MnO2It is raw material, is (1-x) BF-xPT- by chemical formula is prepared
Stoichiometric proportion needed for the BF-PT-BT ternary systems of 0.15BT weighs above-mentioned raw materials, i.e., in control BF-PT-BT ternary systems
Bismuth ferrite：Lead titanates：The ratio between mole of barium titanate is (1-x)：x：0.15, and 0.19≤x≤0.27；It is above-mentioned after by weighing
Raw material is mixed, and obtains that particle is tiny and uniform BF-PT- by grinding at least one times, screening and high-temperature calcination technique
BT synthetic powders；
B. molding biscuit：
The binding agent PVA that mass concentration is not less than 5% is added dropwise in the BF-PT-BT synthetic powders prepared in the step a,
Granulated, binding agent PVA dripping quantities are at least the 7% of BF-PT-BT synthetic powder quality, afterwards by BF- under 100MPa
The compound of PT-BT synthetic powders and binding agent PVA tentatively carries out pressure forming for minimum diameter is 12mm and minimum thickness is
The disk blank of 1mm, then proceeds to few 200MPa isostatic pressings for first base, after isostatic pressed, carries out dumping to first base, most
BF-PT-BT element embryos are obtained afterwards, and binder removal curve is：
First stage since room temperature, is incubated at least 3h, then heat up by 300min after 720min is warming up to 450 DEG C
3h is at least incubated after to 600 DEG C, then furnace cooling completes binder removal process, obtains BF-PT-BT precast body blanks；
C. ceramics are sintered：
Sealed sintering during the BF-PT-BT precast body blanks prepared in the step b are placed on into crucible, sintering curre is：From room
Temperature starts to be warming up to 1100-1200 DEG C with the programming rate of 5 DEG C/min, is then incubated at least 2h, then furnace cooling, final to be obtained
BF-PT-BT ternary system high-temperature piezoelectric ceramic products.
4. the preparation method of bismuth ferrite-lead titanates-barium titanate ternary system high-temperature piezoelectric ceramics according to claim 3, its
It is characterised by：It is as follows by grinding at least one times, screening and high-temperature calcination technique in the step a：According to following material
The ball-milling technology ratio of ball water carries out first time ball milling：
Above-mentioned raw materials after weighing are amounted into 30g to be put into ball grinder, it is that 45g is different to be subsequently adding 30ml deionized waters with weight
Diameter carries out first time ball milling at least 24h with the zirconia ball of shape；
Then first time sieving treatment will be carried out by the slurry obtained after first time ball milling, it is small to leach zirconium oxide by screen cloth
Ball, then slurry is poured into ceramic bowl, the rim of a bowl covering aluminium foil is dried at least 120 DEG C in the baking oven being put into slurry
Dry powder is obtained, after then powder crosses at least mesh screen of 120 mesh, then the powder after sieving is put into crucible is carried out first
Secondary high-temperature calcination synthesizes BF-PT-PT powders, and first time high-temperature calcination process curve is：
The first stage of calcining is to be warming up to 450 DEG C according to the programming rate of at least 5 DEG C/min since room temperature, and insulation is at least
2h, then the second stage calcined, the second stage of calcining are warming up to 750-850 according to the programming rate of at least 5 DEG C/min
DEG C, then at least 4h is incubated, after the second stage for completing calcining, furnace cooling completes first time high-temperature burning process；
After the completion of first time high-temperature calcination, the synthesis powder obtained after first time high-temperature calcination is carried out into grinding again, put
Enter in ball grinder, carry out second ball milling, second ball-milling technology is identical with first time ball-milling technology, by second ball milling
Afterwards, the slurry that will be obtained after ball milling carries out second sieving treatment, and second sieving handling process is processed with first time sieving
Technique is identical, then carry out with second high-temperature calcination of identical of first time high-temperature calcination technique, then carry out again and first time ball
Grinding process identical third time mechanical milling process, discharge drying after third time ball milling, then crosses at least 120 mesh sieves, obtains particle
Tiny and uniform BF-PT-BT synthetic powders.
5. the preparation method of bismuth ferrite-lead titanates-barium titanate ternary system high-temperature piezoelectric ceramics according to claim 3, its
It is characterised by：It is being the BF-PT-BT ternary systems institute of (1-x) BF-xPT-0.15BT by chemical formula is prepared in the step a
When needing stoichiometric proportion to weigh raw material, following numerical relation is also met according to chemical formula：X=1：(0.19~0.23) controls
Lead titanates removes consumption.
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