CN104230333B - A kind of high temperature piezoceramics and preparation method thereof - Google Patents
A kind of high temperature piezoceramics and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of high-curie temperature piezoelectric ceramic, this piezoelectric ceramics formula is (BiYb)1‑xPbxTiyZrx‑yO3+ zmol%A, wherein x=0.91～0.98, y=0.45～0.68, z=0.05～5, A is modifying element.Present invention also offers a kind of method preparing this piezoelectric ceramics, the piezoelectric ceramics utilizing the method to prepare has higher Curie temperature, higher piezoelectric constant, the mechanical quality factor etc. variable compared with low-dielectric loss, higher electromechanical coupling factor and relative broad range, and overcome existing piezoelectric and be difficult to have relatively high-curie temperature and higher pressure electrical property simultaneously, and comprehensive electrical parameter cannot meet specific piezoelectric device and use the problem required.The present invention have technique simple and stable, without special installation, cost is relatively low and is easy to the features such as large-scale industrial production, can be used for corresponding various high temperature piezoelectric device.
Description
Technical field
The present invention relates to electronic ceramics and piezoelectric device field, be specifically related to a kind of piezoelectricity pottery with high-curie temperature
Porcelain and preparation method thereof.
Background technology
The hot environment operation of all kinds of acoustic transducers and vibrating sensor etc. is proposed higher by the development of modern industry
Requirement, this just requires that the piezoelectric that these devices are used has higher Curie temperature (Tc).Such as, at oil
The piezoelectric actuator used on the sound wave well logging transducer of down-hole use, spacecraft and sensor, fuel injection nozzles
The various kinds of sensors etc. that driver and other extreme environments use, is required for using TcMore than 380 DEG C even
Higher piezoelectric ceramics.The T of the most the most frequently used piezoelectric ceramics lead zirconate titanate (PZT)cGenerally significantly less than 360 DEG C.Cause
The gradually depolarization raised with temperature for material and the piezoelectric property degenerate problem caused, its operating temperature upper limit is general
It is at the 1/2 of its Curie temperature, thus the use temperature of PZT is generally significantly less than 180 DEG C.Therefore, research preparation
The piezoelectric ceramics with high-curie temperature is significant to preparing of high temperature piezoelectric device.
It is said that in general, the Curie temperature of piezoelectric is the highest, its piezoelectric property can be the poorest.Such as Publication No.
The Chinese patent of CN1295046 discloses a kind of bismuth laminated piezoelectric ceramic, and its Curie temperature is 865 DEG C, but its pressure
Electrical property is very poor, piezoelectric constant d33The most about 20pC/N.Calendar year 2001 one consists of
(1-x)BiScO3-xPbTiO3(BSPT) perovskite structure piezoelectric ceramics is in the news (Japanse Journal of
Applied Physics, Vol40, pp5999-6002), in this material has preferable piezoelectric property simultaneously and is relatively in
Temperature (when x=0.64, its d33It is about 460pC/N, TcIt is about 450 DEG C).But, raw material Sc2O3Price pole
It is expensive.It addition, this piezoelectric also has comprehensive electrical poor performance (such as mechanical quality factor QmToo low, cause it
Energy consumption is high, use during heating serious), the problem such as unstable properties.This most seriously constrains its actual application.
Therefore, there is high-curie temperature (Tc> 400 DEG C), high piezoelectric constant (d33> 460pC/N) and excellent combination electric property (as
High QmAnd low-loss) the preparation of piezoelectric ceramics and the exploitation of relevant stable technique, always this field is urgently to be resolved hurrily
A difficult problem.
Summary of the invention
Being difficult to obtain high-curie temperature and high tension performance for existing piezoceramic material, comprehensive electrochemical properties cannot simultaneously
Meet device simultaneously and use requirement, or the problem such as expensive, the invention provides one have high-curie temperature,
Higher pressure electrostrictive coefficient, mechanical quality factor are greatly improved and can be in harmonious proportion low new of dielectric loss within the specific limits
Type doping low-cost high-temperature piezoceramic material.
The high-curie temperature piezoelectric ceramic material that the present invention proposes, it has a following chemical structure of general formula:
(BiYb)1-xPbxTiyZrx-yO3+ zmol%A, wherein x span is 0.91～0.98, and y span is
0.45～0.68, z span is 0.05～5, and A is modifying element, can be single metallic element, it is also possible to for
Determination of multiple metal elements.When the ionic radius of this modifying element is less than the ionic radius of the metallic element of Yb and Ti, and it is
During element of multivalence, just there is preferable modifying function, but this modifying element does not include Fe.
Particularly, when one or more during described modifying element is Mn, Nb and Cr element, this piezoelectric ceramics is
There is more preferable combination property.
For preferred system, the span of described x is 0.91～0.98, and y span is 0.45～0.68, z value
Scope is 0.05～5.Piezoelectric ceramics in the range of this has more excellent performance.It is furthermore preferred that the value of described z
Scope is 0.1～2.
The preparation method of described high-curie temperature piezoelectric ceramic comprises the following steps:
(1) by Bi2O3、Yb2O3、Pb3O4、TiO2、ZrO2Claim in molar ratio with oxide or the salt of modifying element
Amount, then mixed grinding obtains material powder；
(2) powder that step (1) obtained dries, sieve after pre-burning, and block pre-burning obtained is fully ground again；
(3) by step (2) grind obtain powder drying, granulation, be aged, sieve after be pressed into ceramic body；
(4) after binder removal, by ceramic body in high temperature sintering at ambient pressure in sealed crucible, piezoelectric ceramic body is prepared；
(5) by the piezoelectric ceramic body polishing burnt till, polishing, by after silver electrode, at 100 DEG C～180 DEG C and 3～5kV/mm
Polarize under electric field.
Preferably, corresponding oxide or the salt of described modifying element includes MnCO3、Nb2O5And Cr2O3。
Lapping mode used by step (1) and step (2) is ball milling.Other compound abrasive modes can also be used, such as machinery
Vibromill；During ball milling, material: abrading-ball: liquid spheres grinding media proportion is about 1:1～2:0.5～2, Ball-milling Time
It is about 6～24 hours.
The calcined temperature of step (2) is 700～900 DEG C, and burn-in time is about 1.5～3 hours.
Bonding agent used by step (3) is the aqueous solution that mass fraction is not more than 6%PVA, and digestion time is little less than 12
Time.
Sintering temperature in step (4) is 1050～1280 DEG C, and sintering time is 2～5 hours.Preferably, sintering temperature
Being 1100～1250 DEG C, sintering time is 2～3 hours
In step (5), poling temperature is 100 DEG C～180 DEG C, and polarized electric field is about 3～5kV/mm, and the time is 20 minutes.
Under this polarization condition, the piezoceramic material prepared has more preferable performance.
The invention provides a kind of composite perofskite with high-curie temperature and integrated piezo excellent performance
(BiYb)1-xPbxTiyZrx-yO3+ zmol%A new type high temperature piezoelectric ceramics, solve existing piezoelectric Curie temperature and
The problem that integrated piezo performance cannot meet the requirement of specific indexes simultaneously.This piezoelectric ceramics has higher height simultaneously
Curie temperature (365～430 DEG C), higher pressure electric constant (170～330pC/N), the variable mechanical quality of relative broad range because of
Number (50～500) and relatively low dielectric loss low (0.001～0.05), can be used for various operating temperature more than 210 DEG C
The dependent piezoelectric device such as transducer, sensor.With other high-temperature piezoelectric ceramic phase ratio, this new piezoelectric ceramics is prepared as
This is much lower, is a kind of very promising high-temperature piezoelectric material.
Accompanying drawing explanation
Fig. 1, (BiYb)0.065Pb0.935Ti0.51Zr0.425O3+ 1.2mol%Mn sinters at 1100 DEG C, is incubated 2.5h institute
Obtain the scanning electron microscope image of sample.
Fig. 2, (BiYb)0.07Pb0.93Ti0.47Zr0.46O3+ 0.1mol%Mn sinters at 1100 DEG C, is incubated 2.5h gained
Jie's temperature collection of illustrative plates of sample.
Detailed description of the invention
Being listed below a preferred embodiment of the present invention, it is used only as explanation of the invention rather than restriction.
Embodiment 1:
By Bi2O3、Yb2O3、Pb3O4、TiO2、ZrO2And MnCO3By (BiYb)0.07Pb0.93Ti0.49Zr0.44O3+
+ 1mol%Mn molar ratio weighing, adds anhydrous ethanol medium mixing and ball milling, dries after sieving in 750 DEG C of pre-burning 2h.
By the ball milling again of block after pre-burning, dry and add 5%PVA granulation, be aged 6 hours, be pressed into a diameter of after sieving
15mm, thickness is the base substrate of about 1.5mm, sinters 2.5h at 1120 DEG C, and gained sample is through polishing, throwing
Light, by after silver, with 4kV/mm electric field polarization 20min in 160 DEG C of silicone oil, after cooling, prepare required ceramics sample,
Test gained comprehensive electrochemical properties is: d33=213pC/N, Tc=395 DEG C, Qm=356, tan δ=0.002.
Embodiment 2:
By Bi2O3、Yb2O3、Pb3O4、TiO2、ZrO2And Nb2O5By (BiYb)0.06Pb0.94Ti0.5Zr0.44O3+
+ 0.2mol%Nb molar ratio weighing, adds aqueous medium mixing and ball milling, dries after sieving in 750 DEG C of pre-burning 2h.Will
Block ball milling again after pre-burning, dry and add 6%PVA granulation, be aged 6 hours, be pressed into a diameter of after sieving
15mm, thickness is the base substrate of about 1.5mm, at 1150 DEG C sinter 3h, gained sample through polishing, polishing,
After silver, with 4kV/mm electric field polarization 10min in 160 DEG C of silicone oil, it is cooled to 110 DEG C of 10min systems that polarize again
Obtaining ceramics sample, test gained comprehensive electrochemical properties is: d33=213pC/N, Tc=390 DEG C, Qm=156, tan δ=0.011.
Embodiment 3:
By Bi2O3、Yb2O3、Pb3O4、TiO2、ZrO2And Cr2O3By (BiYb)0.05Pb0.95Ti0.5Zr0.45O3+
+ 0.2mol%Cr molar ratio weighing, adds aqueous medium mixing and ball milling, dries after sieving in 800 DEG C of pre-burning 2h.Will be pre-
Block ball milling again after burning, dry and add 5%PVA granulation, be aged 6 hours, after sieving, be pressed into a diameter of 15mm,
Thickness is the base substrate of about 1.5mm, sinters 3h at 1150 DEG C, after gained sample is through polishing, polishing, by silver,
With 4kV/mm electric field polarization 10min in 160 DEG C of silicone oil, preparing ceramics sample, test gained comprehensive electrochemical properties is:
d33=220pC/N, Tc=401 DEG C, Qm=180, tan δ=0.001.
Embodiment 4:
By Bi2O3、Yb2O3、Pb3O4、TiO2、ZrO2And Fe2O3By (BiYb)0.055Pb0.945Ti0.48Zr0.465O3+
+ 0.2mol%Fe stoichiometric proportion weighs, and adds anhydrous ethanol medium mixing and ball milling, so that the mixing of all powders is all
Even, dry after sieving in 900 DEG C of pre-burning 2h.Block after pre-burning is carried out abundant ball milling again, dries and add 5%PVA
Granulation, is aged 10 hours, is pressed into a diameter of 12mm after sieving, and thickness is the base substrate of about 1.2mm, in
Sinter 2.5h at 1180 DEG C, prepare required piezoelectric ceramics.Burn till rear sample through polishing, polishing, by silver after,
With 4kV/mm electric field polarization 20min in 120 DEG C of silicone oil, gained ceramics sample comprehensive electrochemical properties is: d33=143pc/N,
Tc=370, Qm=90, tan δ=0.02.The most poor, by the various performance of sample adding Fe seen from this embodiment
It is not suitable for the application of actual high temperature.
Above example premised on technical solution of the present invention under implement, give detailed embodiment and tool
The operating process of body, but protection scope of the present invention is not limited to the above embodiments.
Table 1 gives the composition of more embodiment gained sample, preparation condition, the piezoceramic material for preparing
Structure and performance.
The different composition of ceramics sample of table 1, structure and capabilities list
(being diameter about 12mm, the ceramic disks of thickness about 1mm)
Claims (10)
1. a high temperature piezoceramics, it is characterised in that the chemical structure of general formula of described piezoceramic material is (BiYb)1-xPbxTiyZrx-yO3+ zmol%A, wherein A is modifying element, is the ionic radius multivalent metal element that is less than Yb and Ti ionic radius, but does not include ferro element；In described piezoceramic material general structure, x span is 0.91～0.98, and y span is 0.45～0.68, and z span is 0.05～5.
Piezoceramic material the most according to claim 1, it is characterised in that modifying element used includes one or more in Mn, Nb and Cr.
Piezoceramic material the most according to claim 1 and 2, it is characterised in that in described piezoceramic material, z span is 0.08～2.
4. a preparation method for the arbitrary described piezoelectric ceramics of claims 1 to 3, the method comprises the following steps:
(1) by Bi2O3、Yb2O3、Pb3O4、TiO2、ZrO2Weighing in molar ratio with oxide or the salt of modifying element, then mixed grinding obtains powder；
(2) powder that step (1) obtained dries, sieve after pre-burning, and block pre-burning obtained is fully ground again；
(3) by step (2) grind obtain powder drying, granulation, be aged, sieve after be pressed into ceramic body；
(4) after binder removal, by ceramic body high temperature sintering in sealed crucible, piezoelectric ceramic body is prepared；
(5) by the piezoelectric ceramic body polishing burnt till, polishing, by after silver electrode, polarization under 100 DEG C～180 DEG C and 3～5kV/mm electric fields.
Method the most according to claim 4, it is characterised in that the oxide of described modifying element includes MnCO3、Nb2O5And Cr2O3In one or more.
6. according to the method described in claim 4 or 5, it is characterised in that lapping mode used by step (1) and step (2) is ball milling.
Method the most according to claim 6, it is characterised in that during ball milling, material: abrading-ball: the proportion of liquid spheres grinding media is 1:1～2:0.5～2.
Method the most according to claim 4, it is characterised in that the calcined temperature of step (2) is 700～900 DEG C, burn-in time is 1.5-3 hour.
Method the most according to claim 4, it is characterised in that during step (3) granulation, bonding agent used is the aqueous solution that mass fraction is not more than 6%PVA；Digestion time is not more than 12 hours.
10., according to the method described in claim 4 or 5, it is characterised in that step (4) described sintering temperature is 1050～1280 DEG C, sintering time is 2～5 hours.
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| CN106093302A (en) * | 2016-06-07 | 2016-11-09 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of preparation method promoting metal oxide nano-material air-sensitive performance |
| CN112047756A (en) * | 2020-08-13 | 2020-12-08 | 中国科学院上海硅酸盐研究所 | Method for improving electrical property of ferroelectric/piezoelectric ceramic material |
| CN114075073B (en) * | 2020-08-17 | 2022-12-13 | 中国科学院上海硅酸盐研究所 | PZT-Pb (Sb) 1/2 Nb 1/2 ) Ternary system piezoelectric ceramic material and preparation method and application thereof |
| CN114605150B (en) * | 2022-03-22 | 2023-11-14 | 中山市声诺仪器设备有限公司 | High-density, low-loss and high-dielectric-constant piezoelectric ceramic and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102276248A (en) * | 2011-04-22 | 2011-12-14 | 同济大学 | Oxide up-conversion luminescence piezoelectric material of bismuth lamellar perovskite structure and preparation method thereof |
| CN102299253A (en) * | 2010-06-25 | 2011-12-28 | 富士胶片株式会社 | Piezoelectric film, piezoelectric device and liquid ejection apparatus |
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| CN102299253A (en) * | 2010-06-25 | 2011-12-28 | 富士胶片株式会社 | Piezoelectric film, piezoelectric device and liquid ejection apparatus |
| CN102276248A (en) * | 2011-04-22 | 2011-12-14 | 同济大学 | Oxide up-conversion luminescence piezoelectric material of bismuth lamellar perovskite structure and preparation method thereof |
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| Title |
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| 烧结温度对BiYbO3-PbTiO3-PbZrO3三元系压电陶瓷结构和性能的影响;时亮等;《硅酸盐学报》;20131231;第41卷(第12期);摘要和第1.1节 * |
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