CN102649643B - Niobium lutetium lead plumbate-lead lanthanum zirconate titanate (PLZT) electrooptical ceramics material - Google Patents
Niobium lutetium lead plumbate-lead lanthanum zirconate titanate (PLZT) electrooptical ceramics material Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 20
- 239000000463 material Substances 0.000 title claims abstract description 17
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 4
- SSYBETHNRHYQGU-UHFFFAOYSA-N [Pb].[Lu].[Nb] Chemical compound [Pb].[Lu].[Nb] SSYBETHNRHYQGU-UHFFFAOYSA-N 0.000 title claims abstract description 4
- 229910052746 lanthanum Inorganic materials 0.000 title claims abstract description 4
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 title claims abstract description 4
- 230000007246 mechanism Effects 0.000 claims abstract description 4
- 238000002360 preparation method Methods 0.000 claims description 11
- 238000005245 sintering Methods 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000001354 calcination Methods 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 4
- 239000011230 binding agent Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 238000005469 granulation Methods 0.000 claims description 3
- 230000003179 granulation Effects 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 239000002243 precursor Substances 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims 2
- 238000000227 grinding Methods 0.000 claims 2
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims 2
- 150000001875 compounds Chemical class 0.000 claims 1
- 239000000470 constituent Substances 0.000 claims 1
- HTUMBQDCCIXGCV-UHFFFAOYSA-N lead oxide Chemical compound [O-2].[Pb+2] HTUMBQDCCIXGCV-UHFFFAOYSA-N 0.000 claims 1
- YEXPOXQUZXUXJW-UHFFFAOYSA-N lead(II) oxide Inorganic materials [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 claims 1
- 229910003443 lutetium oxide Inorganic materials 0.000 claims 1
- 239000011812 mixed powder Substances 0.000 claims 1
- 230000010287 polarization Effects 0.000 abstract description 3
- 230000008878 coupling Effects 0.000 abstract description 2
- 238000010168 coupling process Methods 0.000 abstract description 2
- 238000005859 coupling reaction Methods 0.000 abstract description 2
- 238000002050 diffraction method Methods 0.000 abstract 1
- 238000005259 measurement Methods 0.000 abstract 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- 229910010413 TiO 2 Inorganic materials 0.000 description 4
- 239000010955 niobium Substances 0.000 description 4
- 206010013786 Dry skin Diseases 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000001757 thermogravimetry curve Methods 0.000 description 2
- 210000002659 acromion Anatomy 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 238000013480 data collection Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000011363 dried mixture Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000005621 ferroelectricity Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000016507 interphase Effects 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000010587 phase diagram Methods 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 238000001272 pressureless sintering Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
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Abstract
The present invention relates to niobium lutetium lead plumbate-lead lanthanum zirconate titanate (PLZT) electrooptical ceramics material.By powdery diffractometry, scanning electron microscope, dielectric, piezoelectricity and ferroelectric measurement characterize its performance, determine the accurate homotype phase boundary regions of this ternary system.And obtain the component 43Pb (Lu of the optimum performance being positioned at accurate homotype phase battery limit (BL)
1/2nb
1/2) O
3-10PbZrO
3-47PbTiO
3.Its piezo-electric modulus is to d
33=367pC/N, T
c=360 DEG C, electromechanical coupling performance k
p=68%, coercive field E
c=17kv/cm, residual polarization P
r=34.45 μ C/cm
2.Not only can meet the high-tech application such as superpower sensor and Large strain driving mechanism to the requirement of piezoelectric performance, and the high-tech application such as superpower sensor and Large strain driving mechanism can be met to the use temperature requirement of piezoelectric.
Description
Technical field
The present invention relates to the preparation method of a kind of novel piezo-electric ceramic composition and piezoelectric ceramic composition.The chemical formula of this kind of piezoelectric ceramic composition is (1-x-y) Pb (Lu
1/2nb
1/2) O
3-xPbZrO
3-yPbTiO
3, referred to as PLuN-PZ-PT.This kind of material has accurate homotype interphase structure and the Curie temperature Piezoelectric composition material that can match in excellence or beauty with PZT ceramic phase.Belong to function ceramics field.This kind of piezoelectric ceramic composition is suitable as piezoelectric ceramic filter, Piezoelectric Ceramic Oscillator, the piezoelectric ceramic devices such as piezoelectric ceramic vibrator.
Background technology
Ferroelectric/piezoelectric is owing to possessing the excellent advantage such as data-collection performance, fast response time, be widely used in various functional device, as sensor, transverter, sonar, driving mechanism, wave filter, micro-loud speaker etc., in national economy and national defense safety, play irreplaceable vital role.World War II, the U.S., Japan, and USSR (Union of Soviet Socialist Republics) scientist almost finds BaTiO simultaneously
3piezoelectric, the fifties, B.Jaffe found Pb (Zr
1-xti
x) O
3, be called for short PZT.PZT stupalith is the conventional piezoelectric materials that one is widely used in transverter (transducer) and performer (actuator), always dominate in piezoelectricity Application Areas.There is accurate homotype phase boundary in this material.PZT shows piezoelectric property at accurate homotype phase boundary place, the piezoelectric coefficient d of PZT piezoelectric ceramics
33~ 700pC/N, electromechanical coupling factor k
33~ 70%.
But the high (T of PZT ceramic post sintering problem
s> 1250 DEG C), PbO fusing point is lower, and which results in high temperature sintering PZT pottery, it easily departs from ideal composition.In addition, PZT single crystal growing is difficult especially, and up to the present, the growth of the PZT monocrystalline of accurate homotype phase battery limit (BL) remains a difficult problem that cannot overcome.Further, PZT pottery coercive field is relatively little, is not suitable for the use of powerful sensor.
In view of above consideration, a kind ofly can be used for high-power in order to find and have the piezoelectric of high-curie temperature, we have carried out (1-x-y) Pb (Lu
1/2nb
1/2) O
3-xPbZrO
3-yPbTiO
3(PLuN-PZ-PT) research of system solid solution.Have studied ternary system PLuN-PZ-PT accurate homotype phase boundary regions and near the preparation method of component, structure and electric property, for piezoelectricity field provides a kind of novel and can be used for the piezoelectric of the high-curie temperature of high power device.
Summary of the invention
The problem that the object of the invention is to for above-mentioned proposition is found a kind of novel ferroelectric material and studies its preparation technology, grow to solve existing high-curie temperature ferro-electricity single crystal difficulty and be not applicable to the piezoelectric of high power device preferably, for piezoelectric increases a kind of product innovation.This material can be widely used in piezoelectric device field.
A kind of novel piezoelectric ceramic composition material provided by the invention, is characterized in that: chemical constitution is: (1-x-y) Pb (Lu
1/2nb
1/2) O
3-xPbZrO
3-yPbTiO
3, be abbreviated as: PLuN-PZ-PT, belong to typical perovskite structure.Wherein, x=0.1 ~ 0.6, y=0.4 ~ 0.5.There is accurate homotype phase battery limit (BL) in this sosoloid.One of content of the present invention is exactly the position of the accurate homotype phase boundary regions finding out this piezoelectric ceramic composition and studies the associated electrical performance of piezoelectric ceramics of accurate homotype phase boundary regions.
The preparation method of Piezoelectric composition material of the present invention, its preparation method comprises following concrete steps:
A) presoma niobite LuNbO is first prepared
4, preparation method: Lu
2o
3and Nb
2o
5according to metering than weighing, then adding alcohol ball milling 24 hours, then 1150 DEG C of calcinings 1.5 hours, obtaining niobite LuNbO
4.
B) LuNbO is weighed by the stoichiometric ratio of required component
4, TiO
2, ZrO
2, PbO, wherein PbO excessive 3% compensates its volatilization.Then ball milling 24 hours in alcohol and zirconia media.
C) above-mentioned slip, through super-dry (120 DEG C), 800 DEG C of calcinings 6 hours, obtains precursor powder.
D) above-mentioned calcined powder grinds 1.5 hours in mortar, adds the PVA granulation of 5%, compressing tablet, is then warmed up to 500 DEG C with 1.5 DEG C/min, is incubated 2 hours, binder removal.
E) sheet after binder removal is placed on Al
2o
3in crucible, add PbTiO
3in atmosphere material, with 6 ~ 10 DEG C/min ramp to 1170 DEG C, be incubated 2.5 hours, obtain required specimen material.
Accompanying drawing explanation
Fig. 1 is (1-x-y) PLuN-xPZ-yPT piezoceramic material X-ray powder diffraction figure at room temperature prepared by embodiment 1. powder diffractometer model: Rigaku MiniFlex ∏.
Fig. 2 is the transmission electron microscope photo of piezoelectric ceramics sosoloid prepared by embodiment 1.Transmission electron microscope model: JSM6700.
Fig. 3 is the dielectric thermogram after (1-x-y) PLuN-xPZ-yPT piezoelectric polarization of embodiment 1 preparation.Dielectric analysis instrument model: German NovolcontrolAlpha-A.
Fig. 4 is the ferroelectric hysteresis loop of (1-x-y) PLuN-xPZ-yPT piezoelectric under not same electric field prepared by embodiment 1.The model of ferroelectric analyser: aix-ACCTTF2000.
Fig. 5 (1-x-y) Pb (Lu
1/2nb
1/2) O
3-xPbZrO
3-yPbTiO
3ternary phase diagrams and accurate homotype phase boundary.
Embodiment
Below in conjunction with embodiment, the present invention is done further in detail, complete explanation.
Embodiment 1
1. weigh Lu according to stoichiometric ratio
2o
3, Nb
2o
5, add dehydrated alcohol as medium, planetary ball mill 12 hours, 120 DEG C of dryings, 1150 DEG C of calcinings 1.5 hours, obtain presoma LuNbO
4.
2. press general formula (1-x-y) Pb (Lu
1/2nb
1/2) O
3-xPbZrO
3-yPbTiO
3, wherein, x=0.40, y respectively value are 0.40,0.44,0.45,0.46,0.47,0.48,0.50.LuNbO is taken respectively according to stoichiometric ratio
4, ZrO
2, TiO
2.Allow the PbO taking and exceed stoichiometric ratio 3% to compensate the volatilization in its sintering process; Add dehydrated alcohol as medium, planetary ball mill 24 hours.
3. discharging is dry, and dried mixture compressing tablet is loaded Al
2o
3in crucible, 800 DEG C of synthesis 6 hours.
4. pulverize synthetic material, with dehydrated alcohol as medium, planetary ball mill makes it mix in 12 hours again.
5. discharging is dry, adds binding agent PVA (5w%), granulation, makes the sheet of diameter 10mm at the pressure of 20MP, within 6 hours, be warmed up to 500 DEG C, be incubated 2 hours, plastic removal.
6. carry out last sintering.Sintering process 1170 DEG C of pressureless sintering 2.5 hours in oxygen atmosphere, then with furnace temperature cool to room temperature.
7. the PLuN-PZ-PT stupalith Mini-FlexII diffractometer obtained after sintering is carried out material phase analysis, the XRD figure spectrum obtained as shown in Figure 1.Obtained stupalith is pure perovskite structure as seen from Figure 1.
8. Fig. 2 is the photo of the scanning electron microscope of prepared stupalith, and as seen from Figure 2, prepared pottery all presents fine and close microstructure.And along with increasing of PLuN content, density and crystallinity all increase.
9. Fig. 3 is the dielectric thermogram of stupalith under 1Hz ~ 1MHz test frequency of preparation.As can be seen from dielectric spectra, along with the increase of PLuN content, Curie temperature decreases, and presents the acromion of rhombohedral-tetragonal phase change, in addition, and dielectric peak value broadening, dielectric curve frequency of occurrences effect of dispersion.This shows, along with the increase of PLuN content, system Relaxivity strengthens.Dielectric characterization shows that this pottery is a kind of ferroelectric material between normal frroelectrics and relaxation ferroelectric.
10. Fig. 4 is the ferroelectric hysteresis loop of the present embodiment of preparation.As seen from Figure 4, prepared stupalith is compared to PZT stupalith, and it all increases in coercive field Ec and residual polarization Pr.Be applicable on high-power piezoelectric device.
Embodiment 2
1. weigh Lu according to stoichiometric ratio
2o
3, Nb
2o
5, add dehydrated alcohol as medium, planetary ball mill 12 hours, 120 DEG C of dryings, 1150 DEG C of calcinings 1.5 hours, obtain presoma LuNbO
4.
2. press general formula (1-x-y) Pb (Lu
1/2nb
1/2) O
3-xPbZrO
3-yPbTiO
3, wherein, x=0.25, y respectively value are 0.41,0.42,0.43,0.45,0.46,0.47,0.48.LuNbO is taken respectively according to stoichiometric ratio
4, ZrO
2, TiO
2.Allow the PbO taking and exceed stoichiometric ratio 3% to compensate the volatilization in its sintering process; Add dehydrated alcohol as medium, planetary ball mill 24 hours.
3. sintering temperature is set as 1100 DEG C of insulations 2.5 hours.
3. all the other are with embodiment 1.
Embodiment 3
1. weigh Lu according to stoichiometric ratio
2o
3, Nb
2o
5, add dehydrated alcohol as medium, planetary ball mill 12 hours, 120 DEG C of dryings, 1150 DEG C of calcinings 1.5 hours, obtain presoma LuNbO
4.
2. press general formula (1-x-y) Pb (Lu
1/2nb
1/2) O
3-xPbZrO
3-yPbTiO
3, wherein, x=0.10, y respectively value are 0.40,0.43,0.44,0.45,0.46,0.47,0.48,0.50.LuNbO is taken respectively according to stoichiometric ratio
4, ZrO
2, TiO
2.Allow the PbO taking and exceed stoichiometric ratio 3%; Add dehydrated alcohol as medium, planetary ball mill 24 hours.
3. sintering temperature is set as 1020 DEG C of insulations 2.5 hours.
3. all the other are with embodiment 1.
It is important to point out: above embodiment is only used to further illustrate the present invention; can not be interpreted as limiting the scope of the invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.
Claims (3)
1. niobium lutetium lead plumbate-lead lanthanum zirconate titanate (PLZT) electrooptical ceramics material, is characterized in that: the principal constituent compound of described formation is by (1-x-y) Pb (Lu
1/2nb
1/2) O
3-xPbZrO
3-yPbTiO
3represent, in formula, x=0.1 ~ 0.6, y=0.40 ~ 0.50.
2. a preparation method for piezoceramic material according to claim 1, comprises the steps:
(1) first prepare presoma niobite LuNbO4, according to metering than weighing Lu2O3 and Nb2O5, adding alcohol grinding, then calcining 1.5 hours, obtain niobite LuNbO4;
(2) weigh LuNbO4, TiO2, ZrO2, PbO by the stoichiometric ratio of the component of required preparation, wherein PbO excessive 3% compensates its volatilization in sintering process;
(3) above-mentioned mixed powder grinding, slip, through super-dry, after calcining, obtains precursor powder;
(4) powder after calcining grinds again, and granulation, compressing tablet, binder removal, obtains required piezoceramic material after sintering.
3. piezoceramic material according to claim 1 is used for electromechanical transducer, stimulator, electrical condenser, driving mechanism, microwave communication, micro-wave dielectric, wave filter, ultrasonator, energy harvester and piezoelectric buzzer field.
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| CN102817080A (en) * | 2012-09-04 | 2012-12-12 | 中国科学院上海硅酸盐研究所 | Lead lutetioniobate-lead magnesioniobate-lead titanate ternary-system relaxation ferroelectric monocrystal and preparation method thereof |
| CN103011815B (en) * | 2012-12-06 | 2017-10-24 | 中国科学院福建物质结构研究所 | Ternary ferroelectric sosoloid niobium lutetium lead plumbate lead magnesio-niobate lead titanates |
| CN103014863B (en) * | 2012-12-06 | 2018-03-09 | 中国科学院福建物质结构研究所 | Antiferroelectric monocrystalline niobium lutetium lead plumbate and its production and use |
| CN103011816A (en) * | 2012-12-06 | 2013-04-03 | 中国科学院福建物质结构研究所 | Preparation method for binary ferroelectric lead lutecium niobate-lead titanate solid solution |
| CN103011812A (en) * | 2012-12-12 | 2013-04-03 | 中国科学院福建物质结构研究所 | Method for preparing PZN based multi-element composite perovskite type piezoelectric ceramics |
| CN103172373A (en) * | 2012-12-12 | 2013-06-26 | 中国科学院福建物质结构研究所 | Ternary ferroelectric solid solution lead niobate ytterbate-lead zinc niobate-lead titanate |
| CN103641478A (en) * | 2013-11-28 | 2014-03-19 | 中国科学院福建物质结构研究所 | Ferroelectric piezoelectric ceramic material of large-power energy transducer and preparation method thereof |
| CN103710756A (en) * | 2013-12-16 | 2014-04-09 | 中国科学院福建物质结构研究所 | Antiferroelectric crystal lead lutecium niobate-lead titanate and preparation method thereof |
| CN109650888B (en) * | 2018-12-27 | 2019-12-31 | 哈尔滨工业大学 | Low-temperature textured high-electrical-property ternary lead titanate-based relaxor ferroelectric oriented ceramic |
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| Lu et al. | Lead-free piezoelectric ceramics of (Bi 1/2 Na 1/2) TiO 3–(Bi 1/2 K 1/2) TiO 3–(Bi 1/2 Ag 1/2) TiO 3 system |
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