CN107140968A - A kind of high-temp leadless piezoelectric ceramics and preparation method thereof - Google Patents
A kind of high-temp leadless piezoelectric ceramics and preparation method thereof Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims description 10
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 18
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 16
- 230000010287 polarization Effects 0.000 claims abstract description 14
- 238000009768 microwave sintering Methods 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 20
- 238000000498 ball milling Methods 0.000 claims description 20
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 15
- 238000009413 insulation Methods 0.000 claims description 15
- 239000002994 raw material Substances 0.000 claims description 15
- 230000005684 electric field Effects 0.000 claims description 11
- 229910002915 BiVO4 Inorganic materials 0.000 claims description 10
- 125000004122 cyclic group Chemical group 0.000 claims description 10
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 claims description 7
- 229910052573 porcelain Inorganic materials 0.000 claims description 6
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 5
- 229910052593 corundum Inorganic materials 0.000 claims description 5
- 238000005469 granulation Methods 0.000 claims description 5
- 230000003179 granulation Effects 0.000 claims description 5
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 5
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 229910052709 silver Inorganic materials 0.000 claims description 5
- 239000004332 silver Substances 0.000 claims description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 5
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims description 5
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 5
- 238000007493 shaping process Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 8
- 230000028161 membrane depolarization Effects 0.000 abstract description 3
- 230000007547 defect Effects 0.000 description 9
- 239000000463 material Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 238000005259 measurement Methods 0.000 description 6
- 229910002902 BiFeO3 Inorganic materials 0.000 description 5
- 239000000203 mixture Substances 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 230000002411 adverse Effects 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000002305 electric material Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 230000003389 potentiating effect Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
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Abstract
A kind of high-temp leadless piezoelectric ceramics, it is characterised in that constituting formula is：(1‑x)Bi0.96La0.06FeO3‑xBa0.97(Na1/ 2Al1/2)0.03(Cu1/3Ta2/3)O3+0.05BiVO4；WhereinxRepresent molar fraction, 0.05<x<0.4.This ceramics are combined and are prepared from substep synthesis, isostatic pressed, microwave sintering, different voltage type polarization methods, the series of products are environmentally friendly, stability is good, with excellent piezoelectric property, high temperature stability, depolarization temperature is adapted in high-temperature field application more than 500 DEG C.
Description
Technical field
The present invention relates to the lead-free piezoceramic material of high-temperature field application, specifically a kind of ABO3Type perovskite structure
Bi0.96La0.06FeO3Leadless piezoelectric ceramics with high-temperature stability of base and preparation method thereof.
Background technology
High-temperature piezoelectric sensor has fast simple in construction, small volume, response, service life length, by external interference
Small the advantages of, be widely used in atomic energy, Aero-Space, automobile, it is metallurgical with petrochemical industry etc. is industrial shakes
Dynamic and shock measurement.As these industrial circles are fast-developing, the working environment of these electronic equipments is extremely harsh, to pressure
The operating temperature upper limit of electric material it is also proposed higher requirement.Current high-temperature piezoelectric material and device mainly use monocrystalline material
Material, complex manufacturing is expensive, is unfavorable for large-scale application.Piezoelectric ceramics can be prepared into the device of arbitrary shape, system
Standby technique is simple, and cost is relatively low.Therefore, high temperature piezoceramics of the exploitation with excellent properties turn into the task of top priority.
BiFeO3Base piezoelectric ceramic has excellent piezoelectric property and high-temperature stability, while being the unleaded material of environmental protection
Material system, has broad application prospects in high-temperature piezoelectric sensor field.Due to BiFeO3Bi during system ceramic post sintering3+Yi Hui
Hair, Fe3+Ion appraises at the current rate (Fe3+→Fe2+), Lacking oxygen is produced, causes room temperature leakage current big, it is difficult to polarize, so this system is made pottery
Application of the porcelain in piezoelectric field is less.Defect is BiFeO3The key character of base piezoelectric ceramic, is also to determine piezoelectricity ferro
Performance-critical factor.The coupling of the variation of the abutting ion chemistry key of defect, defect and electricdomain, the internal electric field of defect formation
There is obvious influence to the insulating properties of material, piezoelectric property and temperature characterisitic.Meanwhile, doping effect and atmosphere sintering and defect
Generation it is closely related.But these defects are in the unstable characteristic of high temperature, to BiFeO3The piezoelectric property of base piezoelectric ceramic and
High-temperature stability brings adverse effect.Therefore, using the functional effect of defect, optimization defect sturcture, improvement piezoelectric ceramics performance,
Temperature characterisitic and high-temperature electrical conductivity, are an emerging technical supports in current piezoelectric ceramics development.
The content of the invention
The purpose of the present invention is, just to the deficiencies in the prior art, and to provide a kind of high-temp leadless piezoelectric ceramics and its preparation side
Method.This ceramic material has good piezoelectric performance, takes into account high-temperature stability, depolarization temperature >=500oIt is C, environment-friendly
Type, stability are good, piezoelectric property is good, are adapted to 500oUsed under the conditions of C high temperature above.The advantage of this method is preparation technology letter
Single, cost is low.
Realizing the technical scheme of the object of the invention is：
A kind of high-temp leadless piezoelectric ceramics, constituting formula is：
(1-x)Bi0.96La0.06FeO3-xBa0.97(Na1/2Al1/2)0.03(Cu1/3Ta2/3)O3+0.05BiVO4；WhereinxExpression mole
Fraction, 0.05<x<0.4。
The preparation method of above-mentioned high-temp leadless piezoelectric ceramics, comprises the following steps：
(1) first step is with electron level Bi2O3、Fe2O3And La2O3For raw material, according to stoichiometric equation Bi0.96La0.06FeO3Dispensing；
Using absolute ethyl alcohol as medium ball milling 12 hours, dry, then in 720 DEG C of insulations pre-synthesis tripartite distortion in 2 hours in high alumina crucible
The Bi of structure0.96La0.06FeO3Principal crystalline phase；
(2) second step is with electron level Ta2O5、Ba2CO3、CuO、Na2CO3And Al2O3For raw material, according to stoichiometric equation Ba0.97
(Na1/2Al1/2)0.03(Cu1/3Ta2/3)O3Dispensing；Using absolute ethyl alcohol as medium ball milling 12 hours, dry, then in high alumina crucible in
The Ba of 1050 DEG C of insulations, 2 hours pre-synthesis tetragonal distortion structures0.97(Na1/2Al1/2)0.03(Cu1/3Ta2/3)O3Principal crystalline phase；
(3) the 3rd steps are with electron level Bi2O3And V2O5For raw material, according to stoichiometric equation BiVO4Dispensing；Using absolute ethyl alcohol as Jie
Matter ball milling 12 hours, is dried, then in 550 DEG C of insulations, 2 hours pre-synthesis BiVO in high alumina crucible4Principal crystalline phase；
(4) the 4th steps are by synthetic Bi0.96La0.06FeO3、Ba0.97(Na1/2Al1/2)0.03(Cu1/3Ta2/3)O3、BiVO4Powder
Body, according to (1-x)Bi0.96La0.06FeO3-xBa0.97(Na1/2Al1/2)0.03(Cu1/3Ta2/3)O3
+0.05BiVO4Stoichiometric equation dispensing, whereinxRepresent molar fraction, 0.05<x<0.4）；
(5) using absolute ethyl alcohol as medium ball milling 12 hours, dry, add 5% PVA granulations；It is cold etc. quiet under 150Mpa pressure
It is molded；
(6) microwave sintering, 850-900 DEG C is incubated 20 minutes, sinters porcelain, two sides silver-coated electrode into；
(7) polarize, apply 10 cycle sawtooth waveforms cyclic polarizations, then polarized electric field 5000V/mm, frequency 1Hz apply 15
Cycle square wave cyclic polarization, polarized electric field 6000V/mm, frequency 1Hz, 100 DEG C of poling temperature.
This method passes through in BiFeO3A positions add 0.06 La, form stable trigonal crystal structure and distort excessive phase boundary
Constitute Bi0.96La0.06FeO3, add the Ba of low tetragonal distortion structure0.97(Na1/2Al1/2)0.03 (Cu1/3Ta2/3)O3（Wherein A
Compound small ionic radii (the Na of addition1/2Al1/2)2+, formed to be situated between and see tetragonal）, tripartite-cubic quasi- similar shape phase boundary is built, and
The mesoscopic structure of polar nano-microregion is superimposed, band electric domain wall structure is produced, amplifies piezoelectric response；
This method adds BiVO simultaneously4Burning is helped, and compensates A Bi volatilization simultaneously；In conjunction with sawtooth waveforms-square wave cycle of higher pressure
Polarization, while the formation of triggering hole dipole, produces the de- nail effect of domain wall, can produce dipole polarization corresponding with polarity and increase
It is potent with stablizing electricdomain effect, not only to overcome the adverse effect of high temperature charged defects, positive effect can be also produced, therefore,
Piezoelectric property and high-temperature stability can be improved simultaneously.
This method is synthesized using substep, and microwave sintering, sintering temperature is low, and soaking time is short, uniform small grains, fine and close
Degree is high.
This ceramic material has good piezoelectric performance, takes into account high-temperature stability, depolarization temperature >=500oC, environment
Friendly, stability are good, piezoelectric property is good, are adapted to 500oUsed under the conditions of C high temperature above.The advantage of this method is to prepare work
Skill is simple, cost is low.
Embodiment
Present invention is further elaborated with reference to specific embodiment, but is not limitation of the invention.
Embodiment 1：
Prepared composition is：0.96Bi0.96La0.06FeO3-0.04Ba0.97(Na1/2Al1/2)0.03(Cu1/3Ta2/3)O3+0.05BiVO4
High-temp leadless piezoelectric ceramics.
Preparation method comprises the following steps：
(1) first step is with electron level Bi2O3、Fe2O3And La2O3For raw material, according to stoichiometric equation Bi0.96La0.06FeO3Dispensing；
Using absolute ethyl alcohol as medium ball milling 12 hours, dry, then in 720 DEG C of insulations pre-synthesis tripartite distortion in 2 hours in high alumina crucible
The Bi of structure0.96La0.06FeO3Principal crystalline phase；
(2) second step is with electron level Ta2O5、Ba2CO3、CuO、Na2CO3And Al2O3For raw material, according to stoichiometric equation Ba0.97
(Na1/2Al1/2)0.03(Cu1/3Ta2/3)O3Dispensing；Using absolute ethyl alcohol as medium ball milling 12 hours, dry, then in high alumina crucible in
The Ba of 1050 DEG C of insulations, 2 hours pre-synthesis tetragonal distortion structures0.97(Na1/2Al1/2)0.03(Cu1/3Ta2/3)O3Principal crystalline phase；
(3) the 3rd steps are with electron level Bi2O3And V2O5For raw material, according to stoichiometric equation BiVO4Dispensing；Using absolute ethyl alcohol as Jie
Matter ball milling 12 hours, is dried, then in 550 DEG C of insulations, 2 hours pre-synthesis BiVO in high alumina crucible4Principal crystalline phase；
(4) the 4th steps are by synthetic Bi0.96La0.06FeO3、Ba0.97(Na1/2Al1/2)0.03(Cu1/3Ta2/3)O3、BiVO4Powder
Body, according to 0.96Bi0.96La0.06FeO3-0.04Ba0.97(Na1/2Al1/2)0.03(Cu1/3Ta2/3)O3 +0.05BiVO4Stoichiometry
Formula dispensing；
(5) using absolute ethyl alcohol as medium ball milling 12 hours, dry, add 5% PVA granulations；It is cold etc. quiet under 150Mpa pressure
It is molded；
(6) microwave sintering, 850 DEG C are incubated 20 minutes, sinter porcelain, two sides silver-coated electrode into；
(7) polarize, apply 10 sawtooth waveforms cyclic polarizations, then polarized electric field 5000V/mm, frequency 1Hz apply 15 square waves
Cyclic polarization, polarized electric field 6000V/mm, frequency 1Hz, 100 DEG C of poling temperature.
Gained sample carries out piezoelectric property measurement by IRE standards after placing 24 hours to the piezoelectric ceramics being made.Performance is surveyed
Measure result as follows：
| d 33(pC/N) | Qm | k p | εr | tanδ(%) | T d(°C) | T c(°C) |
| 142 | 165 | 0.28 | 582 | 1.05 | 587 | 673。 |
Embodiment 2：
Prepared composition is：0.9Bi0.96La0.06FeO3-0.1Ba0.97(Na1/2Al1/2)0.03(Cu1/3Ta2/3)O3+0.05BiVO4's
High-temp leadless piezoelectric ceramics.
Preparation method comprises the following steps：
(1) first step is with electron level Bi2O3、Fe2O3And La2O3For raw material, according to stoichiometric equation Bi0.96La0.06FeO3Dispensing；
Using absolute ethyl alcohol as medium ball milling 12 hours, dry, then in 720 DEG C of insulations pre-synthesis tripartite distortion in 2 hours in high alumina crucible
The Bi of structure0.96La0.06FeO3Principal crystalline phase；
(2) second step is with electron level Ta2O5、Ba2CO3、CuO、Na2CO3And Al2O3For raw material, according to stoichiometric equation Ba0.97
(Na1/2Al1/2)0.03(Cu1/3Ta2/3)O3Dispensing；Using absolute ethyl alcohol as medium ball milling 12 hours, dry, then in high alumina crucible in
The Ba of 1050 DEG C of insulations, 2 hours pre-synthesis tetragonal distortion structures0.97(Na1/2Al1/2)0.03(Cu1/3Ta2/3)O3Principal crystalline phase；
(3) the 3rd steps are with electron level Bi2O3And V2O5For raw material, according to stoichiometric equation BiVO4Dispensing；Using absolute ethyl alcohol as Jie
Matter ball milling 12 hours, is dried, then in 550 DEG C of insulations, 2 hours pre-synthesis BiVO in high alumina crucible4Principal crystalline phase；
(4) the 4th steps are by synthetic Bi0.96La0.06FeO3、Ba0.97(Na1/2Al1/2)0.03(Cu1/3Ta2/3)O3、BiVO4Powder
Body, according to 0.9Bi0.96La0.06FeO3-0.1Ba0.97(Na1/2Al1/2)0.03(Cu1/3Ta2/3)O3+0.05BiVO4Stoichiometric equation
Dispensing；
(5) using absolute ethyl alcohol as medium ball milling 12 hours, dry, add 5% PVA granulations；It is cold etc. quiet under 150Mpa pressure
It is molded；
(6) microwave sintering, 880 DEG C are incubated 20 minutes, sinter porcelain, two sides silver-coated electrode into；
(7) polarize, apply 10 sawtooth waveforms cyclic polarizations, then polarized electric field 5000V/mm, frequency 1Hz apply 15 square waves
Cyclic polarization, polarized electric field 6000V/mm, frequency 1Hz, 100 DEG C of poling temperature.
Gained sample carries out piezoelectric property measurement by IRE standards after placing 24 hours to the piezoelectric ceramics being made.
Performance measurements are as follows：
| d 33(pC/N) | Qm | k p | εr | tanδ(%) | T d(°C) | T c(°C) |
| 172 | 109 | 0.33 | 625 | 1.16 | 523 | 638。 |
Embodiment 3：
Prepared composition is：0.88Bi0.96La0.06FeO3-0.12Ba0.97(Na1/2Al1/2)0.03(Cu1/3Ta2/3)O3+0.05BiVO4
High-temp leadless piezoelectric ceramics.
Preparation method comprises the following steps：
(1) first step is with electron level Bi2O3、Fe2O3And La2O3For raw material, according to stoichiometric equation Bi0.96La0.06FeO3Dispensing；
Using absolute ethyl alcohol as medium ball milling 12 hours, dry, then in 720 DEG C of insulations pre-synthesis tripartite distortion in 2 hours in high alumina crucible
The Bi of structure0.96La0.06FeO3Principal crystalline phase；
(2) second step is with electron level Ta2O5、Ba2CO3、CuO、Na2CO3And Al2O3For raw material, according to stoichiometric equation Ba0.97
(Na1/2Al1/2)0.03(Cu1/3Ta2/3)O3Dispensing；Using absolute ethyl alcohol as medium ball milling 12 hours, dry, then in high alumina crucible in
The Ba of 1050 DEG C of insulations, 2 hours pre-synthesis tetragonal distortion structures0.97(Na1/2Al1/2)0.03(Cu1/3Ta2/3)O3Principal crystalline phase；
(3) the 3rd steps are with electron level Bi2O3And V2O5For raw material, according to stoichiometric equation BiVO4Dispensing；Using absolute ethyl alcohol as Jie
Matter ball milling 12 hours, is dried, then in 550 DEG C of insulations, 2 hours pre-synthesis BiVO in high alumina crucible4Principal crystalline phase；
(4) the 4th steps are by synthetic Bi0.96La0.06FeO3、Ba0.97(Na1/2Al1/2)0.03(Cu1/3Ta2/3)O3、BiVO4Powder
Body, according to 0.88Bi0.96La0.06FeO3-0.12Ba0.97(Na1/2Al1/2)0.03(Cu1/3Ta2/3)O3 +0.05BiVO4Stoichiometry
Formula dispensing；
(5) using absolute ethyl alcohol as medium ball milling 12 hours, dry, add 5% PVA granulations；It is cold etc. quiet under 150Mpa pressure
It is molded；
(6) microwave sintering, 890 DEG C are incubated 20 minutes, sinter porcelain, two sides silver-coated electrode into；
(7) polarize, apply 10 sawtooth waveforms cyclic polarizations, then polarized electric field 5000V/mm, frequency 1Hz apply 15 square waves
Cyclic polarization, polarized electric field 6000V/mm, frequency 1Hz, 100 DEG C of poling temperature.
Gained sample carries out piezoelectric property measurement by IRE standards after placing 24 hours to the piezoelectric ceramics being made.
Performance measurements are as follows：
| d 33(pC/N) | Qm | k p | εr | tanδ(%) | T d(°C) | T c(°C) |
| 179 | 101 | 0.36 | 711 | 1.12 | 518 | 597。 |
By example given above, present disclosure can be further apparent from, but they are not to this hair
Bright restriction.
Claims (2)
1. a kind of high-temp leadless piezoelectric ceramics, it is characterised in that constituting formula is：
(1-x)Bi0.96La0.06FeO3-xBa0.97(Na1/2Al1/2)0.03(Cu1/3Ta2/3)O3+0.05BiVO4；WhereinxExpression mole
Fraction, 0.05<x<0.4。
2. the preparation method of high-temp leadless piezoelectric ceramics as claimed in claim 1, it is characterised in that comprise the following steps：
（1）The first step is with electron level Bi2O3、Fe2O3And La2O3For raw material, according to stoichiometric equation Bi0.96La0.06FeO3Dispensing；
Using absolute ethyl alcohol as medium ball milling 12 hours, dry, then in 720 DEG C of insulations pre-synthesis tripartite distortion in 2 hours in high alumina crucible
The Bi of structure0.96La0.06FeO3Principal crystalline phase；
（2）Second step is with electron level Ta2O5、Ba2CO3、CuO、Na2CO3And Al2O3For raw material, according to stoichiometric equation Ba0.97
(Na1/2Al1/2)0.03(Cu1/3Ta2/3)O3Dispensing；Using absolute ethyl alcohol as medium ball milling 12 hours, dry, then in high alumina crucible in
The Ba of 1050 DEG C of insulations, 2 hours pre-synthesis tetragonal distortion structures0.97(Na1/2Al1/2)0.03(Cu1/3Ta2/3)O3Principal crystalline phase；
（3）3rd step is with electron level Bi2O3And V2O5For raw material, according to stoichiometric equation BiVO4Dispensing；Using absolute ethyl alcohol as medium
Ball milling 12 hours, is dried, then in 550 DEG C of insulations, 2 hours pre-synthesis BiVO in high alumina crucible4Principal crystalline phase；
（4）4th step is by synthetic Bi0.96La0.06FeO3、Ba0.97(Na1/2Al1/2)0.03(Cu1/3Ta2/3)O3、BiVO4Powder,
According to (1-x)Bi0.96La0.06FeO3-xBa0.97(Na1/2Al1/2)0.03(Cu1/3Ta2/3)O3
+0.05BiVO4Stoichiometric equation dispensing, whereinxRepresent molar fraction, 0.05<x<0.4）；
（5）Using absolute ethyl alcohol as medium ball milling 12 hours, dry, add 5% PVA granulations；The isostatic cool pressing under 150Mpa pressure
Shaping；
（6）Microwave sintering, 850-900 DEG C is incubated 20 minutes, sinters porcelain, two sides silver-coated electrode into；
（7）Polarization, applies 10 cycle sawtooth waveforms cyclic polarizations, then polarized electric field 5000V/mm, frequency 1Hz apply 15
Cycle square wave cyclic polarization, polarized electric field 6000V/mm, frequency 1Hz, 100 DEG C of poling temperature.
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