CN102649643A - Lead lutecium niobate-lead zirconate titanate piezoceramic material - Google Patents
Lead lutecium niobate-lead zirconate titanate piezoceramic material Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 19
- 229910052451 lead zirconate titanate Inorganic materials 0.000 title abstract 2
- OHSVLFRHMCKCQY-UHFFFAOYSA-N lutetium atom Chemical compound [Lu] OHSVLFRHMCKCQY-UHFFFAOYSA-N 0.000 title 1
- 239000000843 powder Substances 0.000 claims abstract description 6
- 239000000919 ceramic Substances 0.000 claims description 18
- 238000002360 preparation method Methods 0.000 claims description 14
- 239000010955 niobium Substances 0.000 claims description 13
- 238000005303 weighing Methods 0.000 claims description 13
- 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 7
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 239000011230 binding agent Substances 0.000 claims description 3
- 238000005469 granulation Methods 0.000 claims description 3
- 230000003179 granulation Effects 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- SSYBETHNRHYQGU-UHFFFAOYSA-N [Pb].[Lu].[Nb] Chemical compound [Pb].[Lu].[Nb] SSYBETHNRHYQGU-UHFFFAOYSA-N 0.000 claims description 2
- 229910052746 lanthanum Inorganic materials 0.000 claims description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 2
- 230000007246 mechanism Effects 0.000 claims description 2
- 239000002243 precursor Substances 0.000 claims description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 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
- 230000015572 biosynthetic process Effects 0.000 claims 1
- 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
- 239000000203 mixture Substances 0.000 abstract description 6
- 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
- 230000010287 polarization Effects 0.000 abstract description 2
- 229910010293 ceramic material Inorganic materials 0.000 abstract 1
- 238000005259 measurement Methods 0.000 abstract 1
- 238000004626 scanning electron microscopy Methods 0.000 abstract 1
- 229910010413 TiO 2 Inorganic materials 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
- 235000019441 ethanol Nutrition 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
- JTCFNJXQEFODHE-UHFFFAOYSA-N [Ca].[Ti] Chemical compound [Ca].[Ti] JTCFNJXQEFODHE-UHFFFAOYSA-N 0.000 description 1
- 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
- 238000012512 characterization method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000004567 concrete Substances 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
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 1
- 230000005621 ferroelectricity Effects 0.000 description 1
- 230000006872 improvement 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
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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Abstract
本发明涉及铌镥酸铅-锆钛酸铅压电陶瓷材料。通过粉末衍射，扫描电镜，介电，压电和铁电测量对其性能进行表征，确定了该三元体系的准同型相界区域。并得到了位于准同型相界区的最佳性能的组分43Pb(Lu1/2Nb1/2)O3-10PbZrO3-47PbTiO3。其压电系数到d33＝367pC/N，Tc＝360℃，机电耦合性能kp＝68％，矫顽场Ec＝17kv/cm，剩余极化Pr＝34.45μC/cm2。不仅可以满足高功率传感器及高应变驱动器等高技术应用对压电材料性能的要求，而且可以满足高功率传感器及高应变驱动器等高技术应用对压电材料的使用温度要求。
The invention relates to a lead niobate lutetate-lead zirconate titanate piezoelectric ceramic material. Its properties were characterized by powder diffraction, scanning electron microscopy, dielectric, piezoelectric and ferroelectric measurements, and the quasi-isomorphic phase boundary region of the ternary system was determined. And the composition 43Pb(Lu 1/2 Nb 1/2 )O 3 -10PbZrO 3 -47PbTiO 3 with the best properties located in the quasi-isomorphic phase boundary region was obtained. Its piezoelectric coefficient is up to d 33 =367pC/N, T c =360°C, electromechanical coupling performance k p =68%, coercive field E c =17kv/cm, remanent polarization P r =34.45μC/cm 2 . It can not only meet the performance requirements of high-tech applications such as high-power sensors and high-strain drivers for piezoelectric materials, but also meet the temperature requirements of high-tech applications such as high-power sensors and high-strain drivers for piezoelectric materials.
Description
Technical field
The present invention relates to the preparation method of a kind of novel piezo-electric ceramic compsn and piezoelectric ceramic composition.The chemical formula of this kind piezoelectric ceramic composition is (1-x-y) Pb (Lu
1/2Nb
1/2) O
3-xPbZrO
3-yPbTiO
3, note by abridging and be PLuN-PZ-PT.This kind material is to have the piezoelectricity composition material that accurate homotype phase boundary structure and Tc can match in excellence or beauty with the PZT ceramic phase.Belong to the function ceramics field.This kind piezoelectric ceramic composition is suitable as piezoelectric ceramic filter, piezoelectric ceramics vibration device, piezoelectric ceramics components and parts such as piezoelectric ceramic vibrator.
Background technology
Ferroelectric/piezoelectric is owing to possess advantages such as good dynamo-electric conversion performance, response speed be fast; Be widely used in various functional devices; Like transmitter, transverter, sonar, driving mechanism, wave filter, little speaker etc., in national economy and national defense safety, bringing into play irreplaceable vital role.During the World War II, the U.S., Japan and the scientist of the FSU almost find BaTiO simultaneously
3Piezoelectric, the fifties, B.Jaffe found Pb (Zr
1-xTi
x) O
3, be called for short PZT.The PZT stupalith is a kind of conventional piezoelectric materials that is widely used in transverter (transducer) and performer (actuator), dominate in the piezoelectricity Application Areas always.There is accurate homotype phase boundary in this material.PZT is the performance 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 ℃), the PbO fusing point is lower, and this has caused high temperature sintering PZT pottery, and it departs from ideal composition easily.In addition, the difficulty that the PZT single crystal growing is special, up to the present, the growth of the PZT monocrystalline of accurate homotype phase battery limit (BL) remains a difficult problem that can't overcome.Also have, PZT pottery coercive field is less relatively, is not suitable for the use of powerful transmitter.
In view of above consideration, a kind ofly can be used for high-power and to have the piezoelectric of high-curie temperature in order to seek, we have carried out (the Lu to (1-x-y) Pb
1/2Nb
1/2) O
3-xPbZrO
3-yPbTiO
3(PLuN-PZ-PT) research of system solid solution.Studied ternary system PLuN-PZ-PT accurate homotype phase boundary region and near preparation method, structure and the electric property of component, for the 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 objective of the invention is to seek a kind of novel ferroelectric material and study its preparation technology to the problem of above-mentioned proposition; To solve the difficult piezoelectric of growing and not being applicable to high power device preferably of existing high-curie temperature ferro-electricity single crystal, for piezoelectric increases a kind of product innovation.This material can be widely used in the piezoelectric device field.
A kind of novel piezoelectric ceramic composition material provided by the invention, it 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 belongs to typical calcium titanium ore 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 to seek out position and the associated electrical performance of studying the piezoelectric ceramics of accurate homotype phase boundary region of the accurate homotype phase boundary region of this piezoelectric ceramic composition.
The preparation method of piezoelectricity composition material of the present invention, its preparation method comprises following concrete steps:
A) at first prepare presoma niobite LuNbO
4, preparation method: Lu
2O
3And Nb
2O
5Than weighing, add the alcohol ball milling then 24 hours according to metering, 1150 ℃ of calcinings 1.5 hours, obtain niobite LuNbO then
4
B) by the stoichiometric ratio weighing LuNbO of required component
4, TiO
2, ZrO
2, PbO, wherein excessive 3% its volatilization of compensation of PbO.Ball milling 24 hours in alcohol and zirconia media then.
C) above-mentioned slip 800 ℃ of calcinings 6 hours, obtains precursor powder through super-dry (120 ℃).
D) above-mentioned calcined powder ground in mortar 1.5 hours, added 5% PVA granulation, and compressing tablet is warmed up to 500 ℃ with 1.5 ℃/min then, is incubated 2 hours, binder removal.
E) sheet after the binder removal is placed on Al
2O
3In the crucible, add PbTiO
3In the atmosphere material, be warmed up to 1170 ℃, be incubated 2.5 hours, obtain required specimen material with 6～10 ℃/min speed.
Description of drawings
Fig. 1 is (1-x-y) PLuN-xPZ-yPT piezoceramic material X-ray powder diffraction figure at room temperature of embodiment 1 preparation. powder diffractometer model: Japanese MiniFlex ∏ of science.
Fig. 2 is the transmission electron microscope photo of the piezoelectric ceramics sosoloid of embodiment 1 preparation.Transmission electron microscope model: JSM6700.
Fig. 3 is the dielectric thermogram after (1-x-y) PLuN-xPZ-yPT piezoelectric of embodiment 1 preparation polarizes.Dielectric analysis appearance model: German Novolcontrol Alpha-A.
Fig. 4 is that (1-x-y) PLuN-xPZ-yPT piezoelectric of embodiment 1 preparation is in different electric ferroelectric hysteresis loop after the match.The model of ferroelectric analyser: aix-ACCT TF2000.
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
The present invention is done further in detail complete explanation below in conjunction with embodiment.
Embodiment 1
1. according to stoichiometric ratio weighing Lu
2O
3, Nb
2O
5, add absolute ethyl alcohol as medium, planetary ball mill 12 hours, 120 ℃ of dryings 1150 ℃ 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 value respectively are 0.40,0.44,0.45,0.46,0.47,0.48,0.50.Take by weighing LuNbO according to stoichiometric ratio respectively
4, ZrO
2, TiO
2Let and take by weighing PbO above stoichiometric ratio 3% to compensate the volatilization in its sintering process; Add absolute ethyl alcohol as medium, planetary ball mill 24 hours.
3. discharging is dry, with the dried mixture compressing tablet Al that packs into
2O
3In the crucible, synthesized 6 hours at 800 ℃.
4. pulverizing synthetic material, as medium, planetary ball mill mixed it in 12 hours once more with absolute ethyl alcohol.
5. discharging is dry, adds sticker PVA (5w%), and granulation presses down the sheet of processing diameter 10mm at the pressure of 20MP, is warmed up to 500 ℃ in 6 hours, is incubated 2 hours, plastic removal.
6. carry out last sintering.Sintering process 1170 ℃ of pressureless sintering 2.5 hours in oxygen atmosphere is then with the furnace temperature cool to room temperature.
7. the PLuN-PZ-PT stupalith that obtains behind the sintering is carried out material phase analysis with the Mini-FlexII diffractometer, the XRD figure spectrum that obtains is as shown in Figure 1.Be pure perovskite structure by the visible institute of Fig. 1 acquisition stupalith.
8. Fig. 2 is the photo of the ESEM of prepared stupalith, and is visible by Fig. 2, and 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.Can find out that from dielectric spectra along with the increase of PLuN content, Curie temperature decreases, and demonstrate the acromion of three parts-cubic phase transformation, in addition, dielectric peak widthization, dielectric curve frequency of occurrences effect of dispersion.This is to show, along with the increase of PLuN content, system relaxation performance strengthens.Dielectric characterization shows that this pottery is a kind of ferroelectric material between normal ferroelectrics and relaxation ferroelectric.
10. Fig. 4 is the ferroelectric hysteresis loop of the present embodiment of preparation.Visible by Fig. 4, prepared stupalith is than the PZT stupalith, and it is all increasing aspect coercive field Ec and the residual polarization Pr.Be applicable on the high-power piezoelectric device.
Embodiment 2
1. according to stoichiometric ratio weighing Lu
2O
3, Nb
2O
5, add absolute ethyl alcohol as medium, planetary ball mill 12 hours, 120 ℃ of dryings 1150 ℃ 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 value respectively are 0.41,0.42,0.43,0.45,0.46,0.47,0.48.Take by weighing LuNbO according to stoichiometric ratio respectively
4, ZrO
2, TiO
2Let and take by weighing PbO above stoichiometric ratio 3% to compensate the volatilization in its sintering process; Add absolute ethyl alcohol as medium, planetary ball mill 24 hours.
3. sintering temperature is set at 1100 ℃ of insulations 2.5 hours.
3. all the other are with embodiment 1.
Embodiment 3
1. according to stoichiometric ratio weighing Lu
2O
3, Nb
2O
5, add absolute ethyl alcohol as medium, planetary ball mill 12 hours, 120 ℃ of dryings 1150 ℃ 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 value respectively are 0.40,0.43,0.44,0.45,0.46,0.47,0.48,0.50.Take by weighing LuNbO according to stoichiometric ratio respectively
4, ZrO
2, TiO
2Let and take by weighing PbO above stoichiometric ratio 3%; Add absolute ethyl alcohol as medium, planetary ball mill 24 hours.
3. sintering temperature is set at 1020 ℃ of insulations 2.5 hours.
3. all the other are with embodiment 1.
It is important to point out: above embodiment only is used for the present invention is further specified; Can not be interpreted as the restriction to protection domain of the present 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 (4)
1. niobium lutetium lead plumbate-lead lanthanum zirconate titanate (PLZT) electrooptical ceramics material, it is characterized in that: the principal constituent compound of said formation is by (1-x-y) Pb (Lu
1/2Nb
1/2) O
3-xPbZrO
3-yPbTiO
3Expression, in the formula, x=0.1～0.6, y=0.40～0.50.
2. piezoceramic material as claimed in claim 1 is characterized in that: there is accurate homotype phase battery limit (BL) in it, and accurate homotype phase region is positioned near y=0.45～0.47; As system component deflection Pb (Lu
1/2Nb
1/2) O
3-xPbTiO
3During one side, accurate homotype phase boundary region broadens.
3. the preparation method of the described piezoceramic material of claim 1 comprises the steps:
(1) at first prepares presoma niobite LuNbO4, than weighing Lu2O3 and Nb2O5, add alcohol and grind, calcined then 1.5 hours, obtain niobite LuNbO4 according to metering;
(2) by the stoichiometric ratio weighing LuNbO4 of the component of required preparation, TiO2, ZrO2, PbO, wherein excessive 3% its volatilization in sintering process of compensation of PbO;
(3) above-mentioned mixed powder grinds, and slip after the calcining, obtains precursor powder through super-dry;
(4) the powder regrinding after the calcining, granulation, compressing tablet obtains required piezoceramic material after the binder removal, sintering.
4. the described piezoceramic material of 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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|---|---|---|---|
| CN201210125316.4A CN102649643B (en) | 2012-04-25 | 2012-04-25 | Niobium lutetium lead plumbate-lead lanthanum zirconate titanate (PLZT) electrooptical ceramics material |
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|---|---|---|---|
| CN201210125316.4A CN102649643B (en) | 2012-04-25 | 2012-04-25 | Niobium lutetium lead plumbate-lead lanthanum zirconate titanate (PLZT) electrooptical ceramics material |
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| Publication Number | Publication Date |
|---|---|
| CN102649643A true CN102649643A (en) | 2012-08-29 |
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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 |
| 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 |
| CN103014863A (en) * | 2012-12-06 | 2013-04-03 | 中国科学院福建物质结构研究所 | Antiferroelectric single crystal lead lutecium niobate, and preparation method and application thereof |
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| CN1511802A (en) * | 2002-12-27 | 2004-07-14 | ���Ĵ���ѧ | Multi-component niobate-based lead-free piezoelectric ceramics |
| EP1669325A1 (en) * | 2004-12-13 | 2006-06-14 | Kerr-McGee Pigments GmbH | Fine Lead-Zirkonium-Titanates and Zirconium-Titanates and method of production using Titaniumdioxide hydrate particles with a specific surface >50 m^2/g |
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| 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 |
| CN103014863A (en) * | 2012-12-06 | 2013-04-03 | 中国科学院福建物质结构研究所 | Antiferroelectric single crystal lead lutecium niobate, and preparation method and application thereof |
| CN103011815A (en) * | 2012-12-06 | 2013-04-03 | 中国科学院福建物质结构研究所 | Ternary ferroelectric solid solution lead lutecium niobate-lead magnesium niobate-lead titanate |
| 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 |
| 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 |
| CN109650888A (en) * | 2018-12-27 | 2019-04-19 | 哈尔滨工业大学 | A kind of high electric property ternary system lead titanate relaxor ferroelectric orientation ceramic of low temperature texture and its preparation method and application |
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| CN102649643B (en) | 2016-03-02 |
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