CN104193334A - Preparation method of PWC-modified PLZT (plomb lanthanum zirconate titanate) piezoelectric ceramic - Google Patents
Preparation method of PWC-modified PLZT (plomb lanthanum zirconate titanate) piezoelectric ceramic Download PDFInfo
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- CN104193334A CN104193334A CN201410332505.8A CN201410332505A CN104193334A CN 104193334 A CN104193334 A CN 104193334A CN 201410332505 A CN201410332505 A CN 201410332505A CN 104193334 A CN104193334 A CN 104193334A
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Abstract
The invention aims at providing a preparation method of Pb(W0.5Cu0.5)O3(PWC)-modified [Pb0.9025La0.065(Zr0.58Ti0.42)0.975Nb0.02O3 (PLZT) piezoelectric ceramic with good electrical performance and high density. The formula of the material is [Pb0.9025La0.065(Zr0.58Ti0.42)0.975Nb0.02O3]+X wt% PWC doped for modification, wherein X is 0-10. The preparation method comprises the following steps: (1), weighing raw materials according to the stoichiometric equation, and preparing PLZT ceramic powder by virtue of a solid-phase synthesis process; (2), pre-sintering the powder prepared in the step (1) at 850 DEG C, and then mixing the powder uniformly and milling into fine powder by virtue of a ball mill; (3), PWC doping and modifying, namely weighing the raw materials according to the stoichiometric equation to prepare PWC, and then adding to the PLZT prepared in the step (2), stirring, drying and grinding to prepare powder; (4), pelletizing the powder prepared in the step (3), tabletting at 500 DEG C and discharging glue; and (5), sintering the pre-sintered ceramic sheet at 950-1150 DEG C for one hour to prepare the PWC-modified PLZT piezoelectric ceramic. The preparation method is simple in process, low in cost and excellent in prepared ceramic performance, and can be used for industrial production of ultrasonic sensors and energy accumulators.
Description
Technical field
The invention belongs to technical field of piezoelectric materials, be specifically related to a kind of cryogenic booster Pb (W
0.5cu
0.5) O
3the preparation method of modification PLZT piezoelectric ceramics, can be for accumulator and sonac.
Background technology
Perovskite structure (ABO
3) PLZT pottery have good ferroelectric, piezoelectric and dielectric properties, thereby be commonly used for accumulator and mini drive.Yet the volatilization that can form imperfect crystal formation and be accompanied by plumbous oxide due to component under high temperature sintering condition can cause stoichiometric equation defect, with traditional sintering method, when sintering temperature is 1200 ℃, be difficult to obtain the PLZT pottery that fine and close sintering is good.In recent years, people are by hot pressed sintering, and the methods such as high-energy ball milling and cryogenic booster can be used successfully in the preparation of PLZT pottery.Can improve ceramic dense degree and electric property with cryogenic booster in traditional these methods of method comparison.This patent adopts PWC ceramic as cryogenic booster modification PLZT: on the one hand because PWC cryogenic booster has lower fusing point, at sintering, can form melting phase acceleration of sintering early stage, contribute to diffusion and the transmission of particle.On the other hand, at sintering later stage W and Cu, can occupy the B position of perovskite structure, can not cause dephasign to generate.The pottery of preparing by the method has very high density, and crystal grain is very thin, structure homogeneous, and electric property is excellent.
Summary of the invention
This patent adopt solid-phase sintering process using PWC as cryogenic booster modification prepare PLZT piezoelectric ceramics.According to stoichiometric equation Pb
0.9025la
0.065(Zr
0.58ti
0.42)
0.975nb
0.02o
3, Pb (W
0.5cu
0.5) O
3prepare ceramic powder, the preparation of raw material drying, raw material weighing, presoma, suspension mixed preparation (PLZT+PWC), grinding, granulation, moulding, sintering, the ceramic grinding burning till, polishing.Crystalline structure divides, shows morphology analysis, density measurement; Polishing sample, roasting polarization of electrode etc., electrical performance testing.
When preparing ceramic powder, add cryogenic booster PWC, addition is 2wt.%～10wt.%, during addition 4wt.%, effect is better, can reduce sintering temperature, promote ceramic densification and reduce microtexture defect, and thering is low dielectric loss and coercive field, can be used as accumulator and sonac.
Accompanying drawing explanation
Fig. 1 is the XRD diffractogram of different components cryogenic booster PWC modification PLZT pottery sintering at 1100 ℃
Fig. 2 is that different components cryogenic booster PWC modification PLZT pottery is schemed at 1100 ℃ of sintered surface SEM
Fig. 3 is the density map of different components cryogenic booster PWC modification PLZT pottery sintering under differing temps
Fig. 4 is the electromechanical coupling factor figure of different components cryogenic booster PWC modification PLZT pottery sintering under differing temps
Fig. 5 is the piezoelectric strain constant figure of different components cryogenic booster PWC modification PLZT pottery sintering under differing temps
Fig. 6 is the mechanical quality factor figure of different components cryogenic booster PWC modification PLZT pottery sintering under differing temps
Fig. 7 is the relative permittivity figure of different components cryogenic booster PWC modification PLZT pottery sintering under differing temps
Fig. 8 is the cryogenic booster PWC modification PLZT pottery of the 4wt.% ferroelectric hysteresis loop figure under different sintering temperatures
Fig. 9 is the dielectric loss figure of different components cryogenic booster PWC modification PLZT pottery sintering at 1100 ℃
Figure 10 is the unit cell parameters table of different components cryogenic booster PWC modification PLZT pottery sintering at 1100 ℃
Embodiment
The preparation method of this kind of PWC modification doping PLZT piezoelectric ceramics, comprises following steps
(1) preparation of PLZT ceramic powder
With analytically pure Pb
3o
4, ZrO
2, TiO
2, La
2o
3, and Nb
2o
5as raw material, according to stoichiometry Pb
0.9025la
0.065(Zr
0.58ti
0.42)
0.975nb
0.02o
3take, mix.By the mixture generating sintering four hours at 850 ℃, sintering 2 hours at 1000 ℃ more afterwards.The powder making packs the nylon ball grinder that contains zirconia balls into, take deionized water as medium ball milling 3 hours.Separating slurry, the PLZT ceramic powder that oven dry is evenly distributed, granularity is thinner.
(2) modification of PWC doping
With analytically pure Cu (NO
3)
23H
2o, Pb (CH
3cOO) 3H
2o and WO
3as raw material, according to stoichiometric equation Pb (W
0.5cu
0.5) O
3take, first by Cu (NO
3)
23H
2o, Pb (CH
3cOO) 3H
2o is dissolved in deionized water, then by WO
3add formation suspension.The PLZT that adds afterwards step (1) to prepare, is uniformly mixed heating, drying simultaneously, the levigate ceramic powder that makes of mortar for the powder that oven dry is obtained.
(3) moulding and the binder removal of pottery
The powder that step (2) is made carries out granulation, adds that the polyvinyl alcohol (5wt.%) that accounts for minute weight 2% grinds again, oven dry, levigate.Then compression moulding, every takes powder 1g, forming pressure 400MPa, 500 ℃ of sintering come unstuck for one hour.
(4) sintering of pottery
By sintering at the ceramic plate of pre-burning and 950 ℃-1150 ℃ a hour, make the PLZT piezoelectric ceramics of PWC modification.
Example
With analytically pure Pb
3o
4, ZrO
2, TiO
2, La
2o
3, Nb
2o
5, Cu (NO
3)
23H
2o, Pb (CH
3cOO) 3H
2o and WO
3as raw material, according to stoichiometry Pb
0.9025la
0.065(Zr
0.58ti
0.42)
0.975nb
0.02o
3, Pb (W
0.5cu
0.5) O
3calculate and take raw material respectively, by above-mentioned steps preparation, obtain the PLZT pottery after modification: for the ease of comparing, the quality of all samples is identical with original size.
Embodiment 1 ceramic composition [Pb
0.9025la
0.065(Zr
0.58ti
0.42)
0.975nb
0.02o
3in]+X wt.%PWC, X gets 0,2,4,6,8,10, and the modification doping of the preparation of PLZT ceramic powder, low-temperature sintering auxiliary agent PWC, the process of shaping-sintering of pottery are according to above-mentioned embodiment step (1), (2), (3), (4).At 1100 ℃, sintering is one hour, measures the crystalline structure of ceramics sample with X-ray diffractometer, and XRD result shows: have typical perovskite structure; Along with the continuous increase of PWC content, at 2 θ angles, be the double diffraction peaks of 45 ° of left and right corresponding be (002) and (200) diffraction peak, the characteristic peak that it is Tetragonal; And unit cell parameters is along with the increase of PWC content increases (with reference to accompanying drawing 1,, Figure 10) gradually.
Embodiment 2 ceramic composition [Pb
0.9025la
0.065(Zr
0.58ti
0.42)
0.975nb
0.02o
3in]+X wt.%PWC, X gets 0,2,4,6,8,10, the process of shaping-sintering of the modification doping of the preparation of PLZT ceramic powder, low-temperature sintering auxiliary agent PWC, pottery is according to above-mentioned embodiment step (1), (2), (3), (4) sintering one hour at 1100 ℃, the pattern that shows with scanning electron microscopy measurement ceramics sample, SEM result shows: along with the increase of doping, pore reduces gradually, sample is dense, even (with reference to the accompanying drawing 2) that surface microstructure size becomes gradually.
Embodiment 3 ceramic composition [Pb
0.9025la
0.065(Zr
0.58ti
0.42)
0.975nb
0.02o
3in]+X wt.%PWC, X gets 0,2,4,6,8,10, sintering temperature has been attempted 950 ℃, 1000 ℃, 1050 ℃, 1100 ℃ and 1150 ℃, sintering time one hour, by Archimedes' principle, measure the density of ceramics sample, result shows: under same sintering temperature, along with the increase of cryogenic booster content, volume density increases gradually, when doping reaches 8%, volume density reaches and is 7.28g/cm to the maximum
3, remaining unchanged afterwards always, state reaches capacity; When cryogenic booster PWC content is identical, along with the raising of sintering temperature, volume density increases (with reference to accompanying drawing 3) gradually.
Embodiment 4 ceramic composition [Pb
0.9025la
0.065(Zr
0.58ti
0.42)
0.975nb
0.02o
3in]+X wt.%PWC, X gets 0,2,4,6,8,10, and at 950-1150 ℃, sintering is one hour, when sintering temperature is lower, and along with the increase of cryogenic booster PWC content, electromechanical coupling factor K
pthere is no too large variation, its value is 0.2; When sintering temperature is greater than 1000 ℃, under same sintering temperature, along with the increase of cryogenic booster PWC content, electromechanical coupling factor k
pincrease gradually; When doping is 4%, electromechanical coupling factor k
preach maximum value; Then along with the increase of cryogenic booster content, electromechanical coupling factor k
pstart to reduce gradually, finally tend towards stability; When one timing of cryogenic booster PWC content, along with the raising of sintering temperature, electromechanical coupling factor k
pincrease gradually by (with reference to accompanying drawing 4).
Embodiment 5 ceramic composition [Pb
0.9025la
0.065(Zr
0.58ti
0.42)
0.975nb
0.02o
3in]+X wt.%PWC, X gets 0,2,4,6,8,10, and at 950-1150 ℃, sintering is one hour, and when sintering temperature is lower, the doping content of cryogenic booster PWC is to piezoelectric coefficient d
33impact little; When sintering temperature is greater than 1050 ℃, cryogenic booster PWC has had remarkably influenced to piezoelectric property; Under same sintering temperature, piezoelectric coefficient d
33along with the increase of doping, increase gradually, when doping is 4%, it is best that performance reaches; Then along with the increase piezoelectric coefficient d of cryogenic booster content
33start to reduce, be finally tending towards gradually constant; Under the cryogenic booster condition of same amount, along with the raising of sintering temperature, piezoelectric coefficient d
33increase gradually, when cryogenic booster content is 4% sintering temperature while being 1150 ℃, piezoelectric coefficient d
33can reach 350pC/N (with reference to accompanying drawing 5).
Embodiment 6[Pb
0.9025la
0.065(Zr
0.58ti
0.42)
0.975nb
0.02o
3in]+X wt.%PWC modification doping, X gets 0,2,4,6,8,10.The modification doping of the preparation of PLZT ceramic powder, low-temperature sintering auxiliary agent PWC, the process of shaping-sintering of pottery are according to above-mentioned embodiment step (1), (2), (3), (4).The amount of PWC has been attempted several situations: 0%, 2%, 4%, 6%, 8%, 10%.When consumption is 4%, over-all properties is best.Sintering temperature has been attempted 950 ℃, 1000 ℃, 1050 ℃, 1100 ℃ and 1150 ℃, sintering time one hour, when sintering temperature is 1050 ℃, the mechanical quality factor of pottery is up to 90, and reduction sintering temperature that can be suitable, energy efficient (with reference to accompanying drawing 6).
Embodiment 7[Pb
0.9025la
0.065(Zr
0.58ti
0.42)
0.975nb
0.02o
3in]+X wt.%PWC modification doping, X gets 0,2,4,6,8,10.The modification doping of the preparation of PLZT ceramic powder, low-temperature sintering auxiliary agent PWC, the process of shaping-sintering of pottery are according to above-mentioned embodiment step (1), (2), (3), (4).By the room temperature dielectric properties of digital electric bridge measure sample, result shows: when cryogenic booster PWC content is constant, and along with the raising of sintering temperature, relative permittivity ε
rincrease gradually; When sintering temperature is 1100 ℃, it is maximum that specific inductivity reaches; When sintering temperature is lower, relative permittivity ε
rless, it is worth lower than 900; When sintering temperature is greater than 1000 ℃, relative permittivity ε
rlarger, more than 1800.When sintering temperature is lower, along with the increase of cryogenic booster doping, relative permittivity ε
rincrease gradually; When sintering temperature is higher, along with the increase of cryogenic booster content, relative permittivity first increases; When content is 4%, ε
rreach and be 2600 (with reference to accompanying drawings 7) to the maximum.
Embodiment 8 ceramic composition [Pb
0.9025la
0.065(Zr
0.58ti
0.42)
0.975nb
0.02o
3in]+X wt.%PWC, X gets sintering one hour at 4,950 ℃, 1000 ℃, 1050 ℃, 1100 ℃ and 1150 ℃, utilizes ferroelectric test macro at room temperature to test the ferroelectric hysteresis loop of sample.Result shows that sample has typical ferroelectric hysteresis loop, along with the increase of cryogenic booster content, remnant polarization P
rfirst increase, when content is 4% maximum, then start to reduce; And coercive field E
cfirst reduce rear increase; The coercive field of sample is all less than 1.2kV/mm (with reference to accompanying drawing 8).
Embodiment 9 ceramic composition [Pb
0.9025la
0.065(Zr
0.58ti
0.42)
0.975nb
0.02o
3in]+X wt.%PWC, X gets at 2,4,6,8,10,11100 ℃ sintering one hour, and the ceramics sample making is done dielectric loss test.Result shows, at probe temperature, during lower than 300 ℃, the equal tan δ of loss of sample is less than 0.05 (with reference to accompanying drawing 9).
Claims (4)
1.Pb (W
0.5cu
0.5) O
3(PWC) preparation method of modification PLZT piezoelectric ceramics, is characterized in that: using PWC as sintering aid, adopt the preparation of solid phase synthesis sintering process.This stupalith has excellent density and less dielectric loss.
2. the preparation method of the PLZT piezoelectric ceramics of PWC modification according to claim 1, is characterized in that: described sintering condition is, sintering temperature is controlled at 950 ℃-1150 ℃, and sintering time is 1 hour.
3. the preparation method of the PLZT piezoelectric ceramics of PWC modification according to claim 1, is characterized in that: the stoichiometric equation of described stupalith is Pb
0.9025la
0.065(Zr
0.58ti
0.42)
0.975nb
0.02o
3.
4. the preparation method of PWC modification PLZT piezoelectric ceramics according to claim 1, is characterized in that: the stoichiometric equation of PWC is Pb (W
0.5cu
0.5) O
3, PWC doping is 2wt.%-10wt.%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113512261A (en) * | 2021-04-23 | 2021-10-19 | 苏州攀特电陶科技股份有限公司 | High-sensitivity piezoelectric composite material for touch feedback and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1674318A (en) * | 2004-03-26 | 2005-09-28 | Tdk株式会社 | Piezoelectric ceramic and piezoelectric device |
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2014
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1674318A (en) * | 2004-03-26 | 2005-09-28 | Tdk株式会社 | Piezoelectric ceramic and piezoelectric device |
Non-Patent Citations (1)
| Title |
|---|
| 陆辉 等: "PLZT压电陶瓷掺杂Pb(W0.5，Cu0.5)O3的研究", 《科技传播》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113512261A (en) * | 2021-04-23 | 2021-10-19 | 苏州攀特电陶科技股份有限公司 | High-sensitivity piezoelectric composite material for touch feedback and preparation method thereof |
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Application publication date: 20141210 |