CN102180665A - Bismuth scandate-lead titanate high-temperature piezoelectric ceramic material and preparation method thereof - Google Patents
Bismuth scandate-lead titanate high-temperature piezoelectric ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a bismuth scandate-lead titanate high-temperature piezoelectric ceramic material. The bismuth scandate-lead titanate high-temperature piezoelectric ceramic material comprises a matrix with the chemical formula of xBiScO3-(1-x)PbTiO3 and bismuth trioxide (Bi2O3) in an amount which is less than 0.4 percent of the total weight of the matrix. The bismuth scandate-lead titanate high-temperature piezoelectric ceramic material is prepared by adding excess Bi2O3 into raw materials of Sc2O3, Bi2O3, Pb3O4 and TiO2 in the metering ratio according to the chemical formula of xBiScO3-(1-x)PbTiO3, wherein x is 0.35 to 0.38; and the using amount of the excess Bi2O3 is 0.1 to 0.4 percent of the total weight of the raw materials of Sc2O3, Bi2O3, Pb3O4 and TiO2 in the metering ratio according to the chemical formula of xBiScO3-(1-x)PbTiO3. The bismuth scandate-lead titanate high-temperature piezoelectric ceramic material solves the problems that ceramic sintering temperature is increased and piezoelectric and dielectric properties are reduced due to deviation of a stoichiometric ratio caused by bismuth volatilization in the sintering process of BSPT ceramic, and has high Curie temperature, excellent piezoelectric property and an actual application value in high-temperature electronic equipment. The invention also discloses a preparation method for the bismuth scandate-lead titanate high-temperature piezoelectric ceramic material. In the preparation method, the piezoelectric ceramic material is prepared by synthesizing and sintering at lower temperature, so production cost is reduced, process steps are simplified, and the material has actual application value.
Description
Technical field
The invention belongs to high-temperature piezoelectric stupalith field, be specifically related to a kind of scandium acid bismuth-lead titanate high-temperature piezoelectric stupalith and preparation method thereof.
Background technology
The high-temperature piezoelectric pottery is widely used in many special dimensions such as aerospace, nuclear energy, metallurgy, petrochemical complex, geological prospecting.As industrial used large power supersonic device, high temp objects ultrasonic applications, the vibration of high temp objects, acceleration and piezometry, built-in shock sensor in the automobile, dynamically fuel injection nozzle etc. all must be selected high-temperature piezoelectric material for use.
The high-temperature piezoelectric material system mainly comprises with the Pb-based lanthanumdoped zirconate titanates being lead base piezoelectric ceramics, niobate lead-free piezoelectric ceramics, various Bi (Me) O bismuth laminated and that develop recently of representative
3-PbTiO
3(Me=Sc, In, Yb...) system.Wherein, the lead base piezoelectric ceramics that with PZT is representative be in all piezoelectric ceramics research the most ripe, use the most successful piezoceramic material, be widely used for making various electronic devices and components.But the Curie temperature of the Pb-based lanthanumdoped zirconate titanates system piezoelectric ceramics of commercial applications is generally at 250-380 ℃ at present, because the hot activation weathering process, its safe handling temperature is limited in 1/2 place of Curie temperature.Only piezoelectric property is good, but use temperature is lower than the requirement that 400 ℃ piezoceramic material can not satisfy current hi-tech development.On the other hand, along with rapid development of science and technology, a lot of electronic and electrical equipments are more and more higher to the requirement of selected piezoelectric ceramic devices use temperature.The piezoelectric that high temperature uses down at first must have high Curie temperature, i.e. not recurring structure phase transformation and influence its piezoelectricity under higher temperature; Secondly the piezoelectric parameter of this material must keep stable in wide temperature range, only in this way could guarantee that piezoelectric device is working properly.Therefore, exploitation has than high-curie temperature, and piezoelectric property is good, and has the piezoelectric of higher resisting temperature aging property just to become the important research direction that develops high-performance, high reliability, wide temperature range piezoelectric ceramic devices.New calcium titanium ore structure ferroelectrics (1-x) BiScO
3-xPbTiO
3(BSPT) the sosoloid system have high Curie temperature, with the equal piezoelectric property of conventional piezoelectric materials PZT, become one of focus of high-temperature piezoelectric material research in recent years.For example by mixing the oxide compound Fe2O of trace
3, Ga
2O
3257 and document J Appl Phys, 2008,103,074116) or add the 3rd urmaterie LiNbO (sees document Sens Actu-A, 2005,122 (A):
3, PbNbO
3(see document Mater Lett, 2008,62,4449 and document J Appl Phys, 2004,95 (1): 231) etc., further improve the BSPT piezoelectric property and improve its Curie temperature.As two constituent element (BiScO
3, PbTiO
3) one of content when higher, BSPT series piezoelectric ceramic material application traditional method also is not easy to synthesize, it is strict to preparation technology, and repeatability is bad.So the someone attempts preparing this material with some novel methods, people such as the Zou Tingting of Tsing-Hua University have improved the piezoelectric property (seeing document Appl Phys Lett, 2008,93,192913) of BSPT pottery significantly by sol-gel method.But this method cost is higher, and the raw material ratio of this material own is expensive in addition, and is not suitable for industrial production.It is (1-x) BiScO that Chinese invention patent prospectus CN101033133A provides composition formula
3-xPb
(1-y)Li
yTi
(1-y)Nb
yO
3Piezoelectric ceramics, its d
33Greater than 380pC/N, k
pGreater than 0.4, T
cGreater than 400 ℃, this pottery adopts the traditional method preparation, and sintering temperature is higher, has increased preparation cost.For the bismuth series ceramic material, the fusing point that bismuth is lower makes it be easy to volatilization in sintering, not only causes ceramic sintering temperature to improve, and also causes pottery to depart from chemical dosage ratio and reduce the piezoelectric ceramics dielectric properties.
Summary of the invention
First purpose of the present invention is to provide a kind of scandium acid bismuth-lead titanate high-temperature piezoelectric stupalith, this material has solved the bismuth volatilization in sintering process of BSPT pottery and has caused chemical dosage ratio to depart from, and the problem that causes ceramic sintering temperature raising and piezoelectricity dielectric properties to descend, it has high Curie temperature and excellent piezoelectric property, has actual using value in high-temperature electronic equipment.
Second purpose of the present invention is to provide the preparation method of above-mentioned scandium acid bismuth-lead titanate high-temperature piezoelectric stupalith, this preparation method adopts lower temperature to synthesize and sintering is made piezoceramic material, reduce production cost, simplified processing step, had actual using value.
First purpose of the present invention is achieved by the following technical solution: a kind of scandium acid bismuth-lead titanate high-temperature piezoelectric stupalith, this material is by being xBiScO at chemical formula
3-(1-x) PbTiO
3Metering than raw material Sc
2O
3, Bi
2O
3, Pb
3O
4And TiO
2In add excessive Bi again
2O
3Prepare, wherein the x value is 0.35-0.38, adds excessive Bi again
2O
3Consumption be xBiScO
3-(1-x) PbTiO
3Metering than the 0.1-0.4% of raw material gross weight.
The value of wherein said x is preferably 0.363, excessive Bi
2O
3Consumption be preferably xBiScO
3-(1-x) PbTiO
3Metering than 0.2% of raw material gross weight.
The present invention adds the excessive oxidation bismuth during by weighing and comes the volatilization of bismuth in the preparation process is effectively compensated, and guarantees the stoichiometric ratio that Low fire ceramic is correct on the one hand, and the interpolation of excessive oxidation bismuth can acceleration of sintering on the other hand, thereby reduces ceramic sintering temperature.The high-temperature piezoelectric stupalith synthetic at a lower temperature and sintering is made has high Curie temperature and excellent piezoelectric property, has actual application value in high-temperature electronic equipment.
Second purpose of the present invention is achieved by the following technical solution: the preparation method of above-mentioned scandium acid bismuth-lead titanate high-temperature piezoelectric stupalith comprises following steps:
(1) presses composition formula xBiScO
3-(1-x) PbTiO
3Stoichiometric ratio take by weighing raw material Sc
2O
3, Bi
2O
3, Pb
3O
4, TiO
2, and add the excessive Bi that accounts for raw material gross weight 0.1-0.4%
2O
3, put into ball grinder, add distilled water, mix and ball milling;
(2) with after the oven dry of the compound behind the ball milling, behind 730-750 ℃ of pre-burning 2-4h, put into ball grinder, add distilled water once more, carry out fine grinding;
(3) add tackiness agent in the porcelain after fine grinding and place mould, be pressed into needed ceramic green sheet;
(4) after 1-3h carries out sintering to 1060-1100 ℃ of insulation with the ceramic green sheet gradient increased temperature, be cooled to room temperature naturally with stove;
(5) on the ceramic plate after will lowering the temperature after the silver electrode, promptly be prepared into the excessive scandium acid bismuth-lead titanate high-temperature piezoelectric stupalith of bismuth after in silicone oil, polarizing.
Wherein, in above-mentioned steps:
The consumption of distilled water is Sc in the step of the present invention (1)
2O
3, Bi
2O
3, Pb
3O
4, TiO
2With excessive Bi
2O
3The 50-70% of raw material gross weight, the rotating speed during ball milling are 100-300 commentaries on classics/min, and the ball milling time is 1-3h.
The bake out temperature of compound is 80-120 ℃ in the step of the present invention (2).
The consumption of distilled water is the 50-70% of the synthetic back of pre-burning powder gross weight in the step of the present invention (2), and the rotating speed during ball milling is 100-300 commentaries on classics/min, and the ball milling time is 3-5h.
Adhesive consumption is the 5-8% of porcelain gross weight behind the ball milling in the step of the present invention (3), and tackiness agent is that weight percentage is the aqueous solution of 5%PVA.
Speed in the step of the present invention (4) during gradient increased temperature is 150-200 ℃/h.
Temperature in the step of the present invention (4) during sintering is preferably 1080 ℃.
After the silver electrode, in 160-180 ℃ silicone oil, the DC electric field that adds the 3-5 kilovoltage by every millimeter thickness of sample polarized 10-20 minute on the ceramic plate in the step of the present invention (5) behind the sintering.
Advantage of the present invention is:
1.. the piezoelectric ceramics of perovskite structure provided by the invention has good piezoelectric property and high Curie temperature, and typical performance perameter is: d
33=380pC/N, k
p=0.484,
Tan δ=0.022, T
c=438 ℃, and do not add the excessive oxidation bismuth and compensate (d
33=308pC/N, k
p=0.43,
Tan δ=0.024, T
c=428 ℃) compare the performance that has improved material significantly;
2.. this stupalith Curie temperature is higher than the PZT piezoelectric ceramics, and piezoelectric property but is on close level with the PZT piezoelectric ceramics, and this material sintering temperature is low, greatly reduces the technology cost;
3.. the high-temperature piezoelectric stupalith of the present invention's preparation can satisfy the requirement that end organs such as piezoceramic transducer, transverter, actuator are used in the hot environment field fully, has the value of practical application in high-temperature electronic equipment.
Description of drawings
Fig. 1 is the piezoelectric property parameters (d of ceramics sample in the specific embodiment of the invention
33, k
p) with excessive Bi
2O
3The changing conditions of addition;
Fig. 2 be ceramics sample in the specific embodiment of the invention the dielectric properties parameter (
Tan δ) with excessive Bi
2O
3The changing conditions of addition;
Fig. 3 is the Curie temperature T of ceramics sample in the specific embodiment of the invention
cWith excessive Bi
2O
3The changing conditions of addition;
Fig. 4 a is excessive Bi in the specific embodiment of the invention
2O
3Addition is the SEM figure of the ceramics sample section of 0wt%;
Fig. 4 b is excessive Bi in the specific embodiment of the invention
2O
3Addition is the SEM figure of the ceramics sample section of 0.2wt%;
Fig. 4 c is excessive Bi in the specific embodiment of the invention
2O
3Addition is the SEM figure of the ceramics sample section of 0.4wt%;
Fig. 5 is that the ceramics sample XRD figure is composed with excessive Bi in the specific embodiment of the invention
2O
3The changing conditions of addition.
Embodiment
The present invention will be described to enumerate a part of specific embodiment below, is necessary to be pointed out that at this following specific embodiment only is used for that the invention will be further described, does not represent limiting the scope of the invention.Some nonessential modifications that other people make according to the present invention and adjustment still belong to protection scope of the present invention.
Embodiment 1
Purchase commercially pure Sc from the market
2O
3, Bi
2O
3, Pb
3O
4, TiO
2As raw material, according to 0.363 BiScO
3-0.637 PbTiO
3Stoichiometric ratio, take by weighing Sc
2O
3, Bi
2O
3, Pb
3O
4, TiO
2, take by weighing again and account for Sc
2O
3, Bi
2O
3, Pb
3O
4And TiO
2The Bi of gross weight 0.1%
2O
3, put into ball grinder, after adding accounted for the distilled water of above-mentioned raw materials gross weight 50%, the rotating speed with 200 commentaries on classics/min on planetary ball mill mixed and levigate 2 hours; To after 100 ℃ of oven dry, be put in the crucible through the compound behind the ball milling, 740 ℃ of pre-burnings, soaking time 2 hours; Powder after pre-burning is synthetic add account for the distilled water of powder gross weight 50% after, with 200 commentaries on classics/min rotating speeds levigate 4 hours; The material that adds suitable amount of adhesive after levigate places mould, is pressed into needed ceramic green sheet, and wherein, tackiness agent is that weight percentage is the aqueous solution of 5% PVA, its consumption be behind the ball milling material heavy 6%; The base sheet is warmed up to 2 hours sintering of 1080 ℃ of insulations by 200 ℃/hour, is cooled to room temperature naturally with stove; Silver electrode on the ceramic plate behind the sintering, in 170 ℃ silicone oil, the DC electric field that adds 4 kilovoltages by every millimeter thickness of sample polarized 10 minutes.
The performance perameter of Zhi Bei high-temperature piezoelectric pottery is as follows according to the method described above: d
33=324pC/N, k
p=0.467,
Tan δ=0.021, T
c=437 ℃.This high-temperature piezoelectric pottery is for being 0.363 BiScO by chemical formula
3-0.637 PbTiO
3Matrix and to account for the matrix gross weight be Bi below 0.4%
2O
3The sosoloid that forms.
Embodiment 2
Scandium acid bismuth-lead titanate high-temperature piezoelectric stupalith that present embodiment provides prepares as follows:
(1) purchases commercially pure Sc from the market
2O
3, Bi
2O
3, Pb
3O
4, TiO
2As raw material, according to 0.363 BiScO
3-0.637PbTiO
3Stoichiometric ratio, take by weighing Sc
2O
3, Bi
2O
3, Pb
3O
4, TiO
2, take by weighing again and account for Sc
2O
3, Bi
2O
3, Pb
3O
4And TiO
2The Bi of gross weight 0.2%
2O
3, be put in the ball grinder, add distilled water, mix and ball milling; Wherein the consumption of distilled water is Sc
2O
3, Bi
2O
3, Pb
3O
4, TiO
260% of raw material gross weight, the rotating speed during ball milling are 100 commentaries on classics/min, and the ball milling time is 2h;
(2) with after the oven dry of the compound behind the ball milling, wherein, the bake out temperature of compound is 100 ℃, behind 740 ℃ of pre-burning 2h, add distilled water once more, the consumption of distilled water is 60% of the synthetic back of a pre-burning powder gross weight, mix and ball milling, the rotating speed during ball milling is 200 commentaries on classics/min, and the ball milling time is 4h;
(3) compound behind the ball milling is added tackiness agent and is placed in the mould, be pressed into needed ceramic green sheet, wherein adhesive consumption be behind the ball milling compound gross weight 6%, tackiness agent is that weight percentage is the aqueous solution of 5%PVA;
(4) ceramic green sheet gradient increased temperature to 1080 a ℃ insulation 2h is carried out sintering after, be cooled to room temperature naturally, wherein gradient increased temperature
The time speed be 200 ℃/h;
(5) on the ceramic green sheet after will lowering the temperature after the silver electrode, in 170 ℃ silicone oil, add the DC electric field polarization 10 minutes of 4 kilovoltages, promptly be prepared into the excessive scandium acid bismuth-lead titanate high-temperature piezoelectric stupalith of bismuth by every millimeter thickness of sample.
The performance perameter of Zhi Bei high-temperature piezoelectric pottery is as follows according to the method described above: d
33=380pC/N, k
p=0.484,
Tan δ=0.022, T
c=438 ℃.This high-temperature piezoelectric pottery is for being 0.363 BiScO by chemical formula
3-0.637 PbTiO
3Matrix and to account for the matrix gross weight be Bi below 0.4%
2O
3The sosoloid that forms.
Embodiment 3
Scandium acid bismuth-lead titanate high-temperature piezoelectric stupalith that present embodiment provides prepares as follows:
(1) purchases commercially pure Sc from the market
2O
3, Bi
2O
3, Pb
3O
4, TiO
2As raw material, according to 0.363 BiScO
3-0.637PbTiO
3Stoichiometric ratio, take by weighing Sc
2O
3, Bi
2O
3, Pb
3O
4, TiO
2, take by weighing again and account for Sc
2O
3, Bi
2O
3, Pb
3O
4And TiO
2The Bi of gross weight 0.3%
2O
3, be put in the ball grinder, add distilled water, mix and ball milling, wherein the consumption of distilled water is Sc
2O
3, Bi
2O
3, Pb
3O
4, TiO
260% of raw material gross weight, the rotating speed during ball milling are 200 commentaries on classics/min, and the ball milling time is 2h;
(2) with after the oven dry of the compound behind the ball milling, bake out temperature is 100 ℃, behind 740 ℃ of pre-burning 2h, add distilled water once more, mix and ball milling, the consumption of distilled water is 60% of the synthetic back of a pre-burning powder gross weight, rotating speed during ball milling is 200 commentaries on classics/min, and the ball milling time is 4h;
(3) compound behind the ball milling is added tackiness agent and be placed in the mould, be pressed into needed ceramic green sheet, wherein tackiness agent is that weight percentage is the aqueous solution of 5%PVA, and adhesive consumption is to account for 6% of compound gross weight behind the ball milling;
(4) ceramic green sheet gradient increased temperature to 1080 a ℃ insulation 2h is carried out sintering after, wherein the speed during gradient increased temperature is 200 ℃/h, is cooled to room temperature naturally;
(5) on the ceramic green sheet after will lowering the temperature after the silver electrode, in 170 ℃ silicone oil, the DC electric field polarization that adds 4 kilovoltages by every millimeter thickness of sample promptly is prepared into the excessive scandium acid bismuth-lead titanate high-temperature piezoelectric stupalith of bismuth after 10 minutes.
The performance perameter of Zhi Bei high-temperature piezoelectric pottery is as follows according to the method described above: performance perameter is: d
33=266pC/N, k
p=0.409,
Tan δ=0.025, T
c=436 ℃.This high-temperature piezoelectric pottery is for being 0.363BiScO by chemical formula
3-0.637 PbTiO
3Matrix and to account for the matrix gross weight be Bi below 0.4%
2O
3The sosoloid that forms.
Scandium acid bismuth-lead titanate high-temperature piezoelectric stupalith that present embodiment provides prepares as follows:
(1) purchases commercially pure Sc from the market
2O
3, Bi
2O
3, Pb
3O
4, TiO
2As raw material, according to 0.363 BiScO
3-0.637PbTiO
3Stoichiometric ratio, take by weighing Sc
2O
3, Bi
2O
3, Pb
3O
4, TiO
2, take by weighing again and account for Sc
2O
3, Bi
2O
3, Pb
3O
4And TiO
2The Bi of gross weight 0.4%
2O
3, be put in the ball grinder, add distilled water, mix and ball milling, wherein the consumption of distilled water is Sc
2O
3, Bi
2O
3, Pb
3O
4, TiO
260% of raw material gross weight, the rotating speed during ball milling are 200 commentaries on classics/min, and the ball milling time is 2h;
(2) with after the oven dry of the compound behind the ball milling, bake out temperature is 100 ℃, behind 740 ℃ of pre-burning 2h, add distilled water once more, mix and ball milling, the consumption of distilled water is 60% of the synthetic back of a pre-burning powder gross weight, rotating speed during ball milling is 200 commentaries on classics/min, and the ball milling time is 4h;
(3) compound behind the ball milling is added tackiness agent and be placed in the mould, be pressed into needed ceramic green sheet, wherein tackiness agent is that weight percentage is the aqueous solution of 5%PVA, the consumption of mixture be behind the ball milling compound gross weight 6%;
(4) ceramic green sheet gradient increased temperature to 1080 a ℃ insulation 2h is carried out sintering after, the speed during gradient increased temperature is 200 ℃/h, is cooled to room temperature naturally;
(5) go up silver electrode on the ceramic green sheet after will lowering the temperature after, in 170 ℃ silicone oil, the DC electric field polarization that adds 4 kilovoltages by every millimeter thickness of sample promptly is prepared into the excessive scandium acid bismuth-lead titanate high-temperature piezoelectric stupalith of bismuth after 10 minutes.
The performance perameter of Zhi Bei high-temperature piezoelectric pottery is as follows according to the method described above: performance perameter is: d
33=210pC/N, k
p=0.377,
Tan δ=0.0229, T
c=445 ℃.This high-temperature piezoelectric pottery is for being 0.363BiScO by chemical formula
3-0.637 PbTiO
3Matrix and to account for the matrix gross weight be Bi below 0.4%
2O
3The sosoloid that forms.
At the foregoing description 1-4, adopt and do not add excessive Bi
2O
3The high-temperature piezoelectric pottery that obtains as a comparison, its concrete preparation method is as follows:
(1) purchases commercially pure Sc from the market
2O
3, Bi
2O
3, Pb
3O
4, TiO
2As raw material, according to 0.363 BiScO
3-0.637PbTiO
3Stoichiometric ratio, take by weighing Sc
2O
3, Bi
2O
3, Pb
3O
4, TiO
2, be put in the ball grinder, wherein, excessive Bi
2O
3Consumption account for Sc
2O
3, Bi
2O
3, Pb
3O
4And TiO
2Gross weight 0.2% adds distilled water, mixes and ball milling, and wherein the consumption of distilled water is Sc
2O
3, Bi
2O
3, Pb
3O
4, TiO
260% of raw material gross weight, the rotating speed during ball milling are 200 commentaries on classics/min, and the ball milling time is 2h;
(2) with after the oven dry of the compound behind the ball milling, bake out temperature is 100 ℃, behind 740 ℃ of pre-burning 2h, add distilled water once more, mix and ball milling, the consumption of distilled water is 60% of the synthetic back of a pre-burning powder gross weight, rotating speed during ball milling is 200 commentaries on classics/min, and the ball milling time is 4h;
(3) compound behind the ball milling is added tackiness agent and be placed in the mould, be pressed into needed ceramic green sheet, wherein tackiness agent is that weight percentage is the aqueous solution of 5%PVA, the consumption of mixture be behind the ball milling compound gross weight 6%;
(4) ceramic green sheet gradient increased temperature to 1080 a ℃ insulation 2h is carried out sintering after, the speed during gradient increased temperature is 200 ℃/h,
Naturally be cooled to room temperature;
(5) go up silver electrode on the ceramic green sheet after will lowering the temperature after, in 170 ℃ silicone oil, the DC electric field polarization that adds 4 kilovoltages by every millimeter thickness of sample promptly is prepared into the excessive scandium acid bismuth-lead titanate high-temperature piezoelectric stupalith of bismuth after 10 minutes.
The performance perameter of Zhi Bei high-temperature piezoelectric pottery is as follows according to the method described above: performance perameter is: d
33=308pC/N, k
p=0.43,
Tan δ=0.024, T
c=428 ℃.This high-temperature piezoelectric pottery is for being 0.363 BiScO by chemical formula
3-0.637 PbTiO
3The sosoloid that forms.
Purchase commercially pure Sc from the market
2O
3, Bi
2O
3, Pb
3O
4, TiO
2As raw material, according to 0.35 BiScO
3-0.65 PbTiO
3Stoichiometric ratio, take by weighing Sc
2O
3, Bi
2O
3, Pb
3O
4, TiO
2, take by weighing again and account for Sc
2O
3, Bi
2O
3, Pb
3O
4And TiO
2The Bi of gross weight 0.15%
2O
3, being put in the ball grinder, after adding accounted for the distilled water of above-mentioned raw materials gross weight 50%, the rotating speed with 150 commentaries on classics/min on planetary ball mill mixed and levigate 3 hours; To after 90 ℃ of oven dry, be put in the crucible through the compound behind the ball milling, 730 ℃ of pre-burnings, soaking time 3 hours; Add in the powder after pre-burning is synthetic account for the distilled water of powder gross weight 50% after, with 250 commentaries on classics/min rotating speeds levigate 3 hours; The material that adds suitable amount of adhesive (weight percentage is the aqueous solution of 5%PVA, and consumption is heavy by 7% for material) after levigate places mould, is pressed into needed ceramic green sheet; The base sheet is warmed up to 2.5 hours sintering of 1090 ℃ of insulations by 180 ℃/hour, is cooled to room temperature naturally with stove; Silver electrode on the ceramic plate behind the sintering, in 160 ℃ silicone oil, the DC electric field that adds 4.5 kilovoltages by every millimeter thickness of sample polarized 15 minutes.
The performance perameter of Zhi Bei high-temperature piezoelectric pottery is as follows according to the method described above: performance perameter is: d
33=351pC/N, k
p=0.472,
Tan δ=0.022, T
c=430 ℃.This high-temperature piezoelectric pottery is for being 0.363BiScO by chemical formula
3-0.637 PbTiO
3Matrix and to account for the matrix gross weight be Bi below 0.4%
2O
3The sosoloid that forms.
Embodiment 6
Purchase commercially pure Sc from the market
2O
3, Bi
2O
3, Pb
3O
4, TiO
2As raw material, according to 0.38 BiScO
3-0.62 PbTiO
3Stoichiometric ratio, take by weighing Sc
2O
3, Bi
2O
3, Pb
3O
4, TiO
2, take by weighing again and account for Sc
2O
3, Bi
2O
3, Pb
3O
4And TiO
2The Bi of gross weight 0.35%
2O
3, being put in the ball grinder, after adding accounted for the distilled water of above-mentioned raw materials gross weight 65%, the rotating speed with 250 commentaries on classics/min on planetary ball mill mixed and levigate 1.5 hours; To after 110 ℃ of oven dry, be put in the crucible through the compound behind the ball milling, 750 ℃ of pre-burnings, soaking time 2.5 hours; Powder after pre-burning is synthetic add account for the distilled water of powder gross weight 65% after, with 150 commentaries on classics/min rotating speeds levigate 4 hours; The material that adds suitable amount of adhesive (weight percentage is the aqueous solution of 5%PVA, and consumption is heavy by 6.5% for material) after levigate places mould, is pressed into needed ceramic green sheet; The base sheet is warmed up to 2.5 hours sintering of 1090 ℃ of insulations by 190 ℃/hour, is cooled to room temperature naturally with stove; Silver electrode on the ceramic plate behind the sintering, in 170 ℃ silicone oil, the DC electric field that adds 3 kilovoltages by every millimeter thickness of sample polarized 15 minutes.
The performance perameter of Zhi Bei high-temperature piezoelectric pottery is as follows according to the method described above: performance perameter is: d
33=233pC/N, k
p=0.392,
Tan δ=0.023, T
c=442 ℃.This high-temperature piezoelectric pottery is for being 0.363BiScO by chemical formula
3-0.637 PbTiO
3Matrix and to account for the matrix gross weight be Bi below 0.4%
2O
3The sosoloid that forms.
Embodiment 7
Purchase commercially pure Sc from the market
2O
3, Bi
2O
3, Pb
3O
4, TiO
2As raw material, according to 0.37 BiScO
3-0.63 PbTiO
3Stoichiometric ratio, take by weighing Sc
2O
3, Bi
2O
3, Pb
3O
4, TiO
2, take by weighing again and account for Sc
2O
3, Bi
2O
3, Pb
3O
4And TiO
2The Bi of gross weight 0.25%
2O
3, being put in the ball grinder, after adding accounted for the distilled water of above-mentioned raw materials gross weight 70%, the rotating speed with 200 commentaries on classics/min on planetary ball mill mixed and levigate 2 hours; To after 100 ℃ of oven dry, be put in the crucible through the compound behind the ball milling, 750 ℃ of pre-burnings, soaking time 2.5 hours; Powder after pre-burning is synthetic add account for the distilled water of powder gross weight 70% after, with 200 commentaries on classics/min rotating speeds levigate 4 hours; The material that adds suitable amount of adhesive (weight percentage is the aqueous solution of 5%PVA, and consumption is heavy by 5% for material) after levigate places mould, is pressed into needed ceramic green sheet; The base sheet is warmed up to 3 hours sintering of 1060 ℃ of insulations by 160 ℃/hour, is cooled to room temperature naturally with stove; Silver electrode on the ceramic plate behind the sintering, in 170 ℃ silicone oil, the DC electric field that adds 4 kilovoltages by every millimeter thickness of sample polarized 10 minutes.
The performance perameter of Zhi Bei high-temperature piezoelectric pottery is as follows according to the method described above: performance perameter is: d
33=318pC/N, k
p=0.448,
Tan δ=0.0234, T
c=428 ℃.This high-temperature piezoelectric pottery is for being 0.363 BiScO by chemical formula
3-0.637 PbTiO
3Matrix and to account for the matrix gross weight be Bi below 0.4%
2O
3The sosoloid that forms.
With chemical formula in embodiment 1-4 and the control sample is 0.363 BiScO
3-0.637 PbTiO
3Matrix and to account for the matrix gross weight be Bi below 0.4%
2O
3The high-temperature piezoelectric pottery that forms is an example, has carried out performance test, and the result is as follows:
From accompanying drawing 1 as can be seen, excessive Bi
2O
3When addition is 0.2wt%, the piezoelectric property parameters (d of ceramics sample
33, k
p) the best.
From accompanying drawing 2 as can be seen, excessive Bi
2O
3When addition is 0.2wt%, the specific inductivity of ceramics sample
Maximum, and dielectric loss tan δ is less.
From accompanying drawing 3, as can be seen, and do not add the ceramics sample that the excessive oxidation bismuth compensates and compare excessive interpolation 0.2wt%Bi
2O
3The time, the Curie temperature T of ceramics sample
cIncrease.
From accompanying drawing 4a-4c, as can be seen, do not adding excessive Bi
2O
3The time, there is increased number of stomata in the ceramics sample of formation, grain size is inhomogeneous; Add the excessive Bi of 0.2wt%
2O
3The grain-size of pottery increases to some extent, and pore is few, and crystal boundary is clear, the even structure densification; As the excessive Bi of further increase
2O
3During to 0.4wt%, ceramic crystalline grain diminishes, and more space occurs, and it is comparatively fuzzy that crystal boundary also becomes, and defective is more in the ceramic structure.The performance perameter of this and ceramics sample is with Bi
2O
3The Changing Pattern unanimity of addition.
From accompanying drawing 5, as can be seen, add excessive Bi
2O
3, principal crystalline phase still keeps single perovskite structure.Along with excessive Bi
2O
3Increase from 0 to 0.2wt%, the intensity of diffraction peak strengthen gradually and 45 ° near the diffraction peak of two broadenings become obvious gradually.Along with the excessive Bi of further increase
2O
3During to 0.4wt%, diffraction peak begin not only to weaken and 45 ° near the diffraction peak swarming but also become so unobvious, near micro-rich bismuth phase (in the collection of illustrative plates 2 θ=28.3 ° shown in the asterisk) appears in the system simultaneously.The performance perameter of this and ceramics sample is with Bi
2O
3The Changing Pattern unanimity of addition.
Claims (10)
1. scandium acid bismuth-lead titanate high-temperature piezoelectric stupalith is characterized in that: this material is by being xBiScO at chemical formula
3-(1-x) PbTiO
3Metering than raw material Sc
2O
3, Bi
2O
3, Pb
3O
4And TiO
2In add excessive Bi again
2O
3Prepare, wherein the x value is 0.35-0.38, the more excessive Bi of Jia Ruing
2O
3Consumption be xBiScO
3-(1-x) PbTiO
3Metering than the 0.1-0.4% of raw material gross weight.
2. scandium acid bismuth according to claim 1-lead titanate high-temperature piezoelectric stupalith, it is characterized in that: the value of described x is 0.363, excessive Bi
2O
3Consumption be xBiScO
3-(1-x) PbTiO
3Metering than 0.2% of raw material gross weight.
3. the preparation method of claim 1 or 2 described scandiums acid bismuth-lead titanate high-temperature piezoelectric stupaliths is characterized in that: comprise following steps:
(1) presses composition formula xBiScO
3-(1-x) PbTiO
3Stoichiometric ratio take by weighing raw material Sc
2O
3, Bi
2O
3, Pb
3O
4, TiO
2, and add the excessive Bi that accounts for raw material gross weight 0.1-0.4%
2O
3, put into ball grinder, add distilled water, mix and ball milling;
(2) with after the oven dry of the compound behind the ball milling, behind 730-750 ℃ of pre-burning 2-4h, put into ball grinder, add distilled water once more, carry out fine grinding;
(3) add tackiness agent in the porcelain after fine grinding and place mould, be pressed into needed ceramic green sheet;
(4) after 1-3h carries out sintering to 1060-1100 ℃ of insulation with the ceramic green sheet gradient increased temperature, be cooled to room temperature naturally with stove;
(5) silver electrode on the ceramic plate after will lowering the temperature promptly is prepared into the excessive scandium acid bismuth-lead titanate high-temperature piezoelectric stupalith of bismuth after polarizing in silicone oil.
4. the preparation method of scandium acid bismuth according to claim 3-lead titanate high-temperature piezoelectric stupalith, it is characterized in that: the consumption of distilled water is Sc in the step (1)
2O
3, Bi
2O
3, Pb
3O
4, TiO
2With excessive Bi
2O
3The 50-70% of raw material gross weight, the rotating speed during ball milling are 100-300 commentaries on classics/min, and the ball milling time is 1-3h.
5. the preparation method of scandium acid bismuth according to claim 3-lead titanate high-temperature piezoelectric stupalith, it is characterized in that: the bake out temperature of compound is 80-120 ℃ in the step (2).
6. the preparation method of scandium acid bismuth according to claim 3-lead titanate high-temperature piezoelectric stupalith, it is characterized in that: the consumption of distilled water is the 50-70% of the synthetic back of pre-burning powder gross weight in the step (2), rotating speed during ball milling is 100-300 commentaries on classics/min, and the ball milling time is 3-5h.
7. the preparation method of scandium acid bismuth according to claim 3-lead titanate high-temperature piezoelectric stupalith, it is characterized in that: adhesive consumption is the 5-8% of porcelain gross weight behind the ball milling in the step (3), and tackiness agent is that weight percentage is the aqueous solution of 5%PVA.
8. the preparation method of scandium according to claim 3 acid bismuth-lead titanate high-temperature piezoelectric stupalith is characterized in that: the speed in the step (4) during gradient increased temperature is 150-200 ℃/h.
9. the preparation method of scandium according to claim 3 acid bismuth-lead titanate high-temperature piezoelectric stupalith is characterized in that: the temperature in the step (4) during sintering is 1080 ℃.
10. the preparation method of scandium acid bismuth according to claim 3-lead titanate high-temperature piezoelectric stupalith, it is characterized in that: on the ceramic plate in the step (5) behind the sintering after the silver electrode, in 160-180 ℃ silicone oil, the DC electric field that adds the 3-5 kilovoltage by every millimeter thickness of sample polarized 10-20 minute.
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