WO2017114741A1 - Matériau céramique bisco3-pbtio3 piézoélectrique à haute température chimiquement modifié pour une réponse en tension améliorée, et procédé pour obtenir ledit matériau céramique - Google Patents

Matériau céramique bisco3-pbtio3 piézoélectrique à haute température chimiquement modifié pour une réponse en tension améliorée, et procédé pour obtenir ledit matériau céramique Download PDF

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Publication number
WO2017114741A1
WO2017114741A1 PCT/EP2016/082337 EP2016082337W WO2017114741A1 WO 2017114741 A1 WO2017114741 A1 WO 2017114741A1 EP 2016082337 W EP2016082337 W EP 2016082337W WO 2017114741 A1 WO2017114741 A1 WO 2017114741A1
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ceramic material
piezoelectric ceramic
piezoelectric
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procedure
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Miguel ALGUERÓ GIMÉNEZ
Harvey AMORÍN GONZÁLEZ
Alicia CASTRO LOZANO
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Consejo Superior de Investigaciones Cientificas CSIC
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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N30/00—Piezoelectric or electrostrictive devices
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N30/00—Piezoelectric or electrostrictive devices
    • H10N30/80—Constructional details
    • H10N30/85—Piezoelectric or electrostrictive active materials
    • H10N30/853—Ceramic compositions
    • H10N30/8548—Lead-based oxides
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
    • C04B35/462—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates
    • C04B35/472—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on lead titanates
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N30/00—Piezoelectric or electrostrictive devices
    • H10N30/01—Manufacture or treatment
    • H10N30/09—Forming piezoelectric or electrostrictive materials
    • H10N30/093—Forming inorganic materials
    • H10N30/097—Forming inorganic materials by sintering

Definitions

  • the invention relates to a high temperature piezoelectric BiSc0 3 -PbTi0 3 ceramic material of formula Bi 1 -x+ 2 y Pb x- 3 y Sc 1-x Ti x 0 3 , wherein x ranges from 0.64 to 0.68 and y ranges from 0.01 to 0,025, which includes a point defect engineering for enhanced voltage response. Furthermore, the invention refers to a procedure for obtaining said ceramic material by conventional sintering of nanocrystalline powders synthesized by mechanochemical activation of a stoichiometric mixture of precursors. Finally, the invention also relates to the use of the chemically engineered BiSc0 3 -PbTi0 3 ceramic material as part of sensing devices and magnetic sensing devices.
  • BiSc0 3 -PbTi0 3 is the most promising system among general formula BiM0 3 -PbTi0 3 , wherein M is a trivalent cation in octahedral coordination, perovskite solid solutions with enhanced electromechanical response at ferroelectric morphotropic phase boundaries (MPB), and high Curie temperature.
  • M is a trivalent cation in octahedral coordination
  • MPB ferroelectric morphotropic phase boundaries
  • This material is being extensively investigated as an alternative to state of the art Pb(Zr,Ti)0 3 (PZT) for expanding the operation temperature of high sensitivity piezoelectric ceramics beyond 200°C up to 400°C.
  • the binary system (1 -x)BiSc0 3 -xPbTi0 3 presents a MPB between ferroelectric polymorphic phases of rhombohedral R3m and tetragonal PAmm symmetry at x ⁇ 0.64, composition for which the Curie temperature T c is « 450°C, while piezoelectric coefficients d 33 of -450 pC N "1 are typically achieved after poling.
  • This T c is 100°C above that of Pb(Zr,Ti)0 3 , likewise d 33 that also significantly exceeds the figure of « 245 pC N "1 for ceramics of the latter material at its own MPB.
  • the charge piezoelectric coefficient is comparable to those of available commercial high sensitivity piezoelectric ceramics of chemically engineered PZT.
  • BiSc0 3 -PbTi0 3 cannot be directly used in most applications. This is the case of sensing technologies like accelerometers, vibration monitoring, hydrophones or magnetic field sensors, for which the voltage piezoelectric coefficient g 33 rather than the charge piezoelectric coefficient d 33 is the key parameter. This coefficient is equal to d 33 times the reciprocal permittivity that is very low (or the permittivity very high) in poled BiSc0 3 -PbTi0 3. Therefore, and for the reasons stated above, it is needed to develop new BiSc0 3 -PbTi0 3 materials, optimized for specific applications.
  • the present invention discloses a perovskite piezoelectric BiSc0 3 -PbTi0 3 material of formula Bi 1-x+2y Pb x-3y Sc 1-x Ti x 0 3 , wherein x ranges from 0.64 to 0.68 and y ranges from 0.01 to 0.025, which exhibits an enhanced electrochemical response at a perovskite morphotropic phase boundary between polymorphs of rhombohedral R3m and tetragonal PAmm symmetries, high Curie temperature, and a point defect engineering for enhanced voltage response.
  • the high temperature, high sensitivity and enhanced voltage response piezoelectric ceramic of the present invention is a dense, and highly homogenous fine grained microstructure with an average grain size that can be tailored from 1 .0 ⁇ up to 2.5 ⁇ .
  • the present invention discloses a procedure for obtaining said ceramic material that refers to its preparation by conventional sintering of nanocrystalline powders synthesized by mechanochemical activation of precursors in a high energy planetary mill.
  • This procedure based on highly reactive powders, allows the suppression of Bi 2 0 3 and PbO volatilization during the high temperature sintering, so that stoichiometric mixtures of the precursors (Bi 2 0 3 , Sc 2 0 3 , PbO, Ti0 2 and Mn 2 0 3 ) can be used, while avoiding the necessity of controlling the atmosphere during the final thermal treatment by burying the green bodies in powder during the sintering.
  • a first aspect of the present invention relates to a piezoelectric ceramic material characterized in that it has
  • the piezoelectric ceramic material of the present invention has perovskite single phase placed at a morphotropic phase boundary between polymorphs of rhombohedral R3m and tetragonal PAmm symmetries that is the responsible for the high piezoelectric response and, moreover, it includes an engineered point defect for enhanced voltage response that makes the material suitable to be used in sensing technologies.
  • engineered point defect refers to a point defect that is introduced at or around a single lattice point of the perovskite, concretely by the controlled substitution of Bi 3+ for Pb 2+ in the A-site (cuboctahedral coordination) of the AB0 3 perovskite, along with the formulation of one Pb vacancy per each two substitutions for charge compensation.
  • This controlled substitution that does not require additional chemical species, but the introduction of an A-site non-stoichiometry, results in significant lattice stiffening and thus, a decrease of the dielectric permittivity and elastic compliance. Moreover, this is achieved while the material is maintained at the morphotropic phase boundary between polymorphs of rhombohedral R3m and tetragonal PAmm symmetries, known to be required for high piezoelectric response.
  • the piezoelectric ceramic material of the present invention has a dense and homogeneous fine grained microstructure with average grain size of between 1 .0 ⁇ and 1 .5 ⁇ .
  • a second aspect of the present invention relates to a procedure for obtaining the piezoelectric ceramic material mentioned above, characterized in that it comprises the following steps:
  • Step (a) is preferably performed in a planetary mill at 300 rpm for 20 h.
  • step (a) is performed for the synthesis of a nanocrystalline powder of formula Bi 1-x+ 2yPb x- 3 y Sci- x Ti x 0 3 , wherein x is 0.64 and y is 0.01 .
  • a third aspect of the invention refers to a piezoelectric ceramic composite comprising ⁇ the piezoelectric ceramic material according to any of claims 1 to 3;
  • magneticstrictive material refers to a ferromagnetic material that changes its shape or dimensions during the process of magnetization.
  • the magnetostrictive material that forms the piezoelectric ceramic composite is selected from the list consisting of Terfenol-D, Metglass, spinel oxides of formula AFe 2 0 4 , wherein A is Ni, Co or a combination thereof, and a combination thereof.
  • the piezoelectric ceramic composite mentioned above is of particulate, fiber or laminate type.
  • Another aspect of the present invention refers to the use of the piezoelectric ceramic material as described above, as part of a sensing device.
  • sensing devices are accelerometers, vibration monitoring or hydrophones.
  • the piezoelectric ceramic material of the present invention is the active element in these sensing technologies.
  • the last aspect of the invention refers to the use of the piezoelectric ceramic composite described above as part of a magnetic sensing device such as a magnetic transducer.
  • the piezoelectric ceramic composite of the present invention comprising the piezoelectric ceramic material of the present invention and a magnetostrictive material, is the active element in magnetic sensing technologies.
  • all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skilled in the art to which this invention belongs. Methods and materials similar or equivalent to those described herein can be used in the practice of the present invention.
  • the word "comprise” and its variations are not intended to exclude other technical features, additives, components, or steps. Additional objects, advantages and features of the invention will become apparent to those skilled in the art upon examination of the description or may be learned by practice of the invention.
  • the following examples and drawings are provided by way of illustration and are not intended to be limiting of the present invention.
  • nanocrystalline powder was uniaxially pressed into 12 mm diameter pellets, which were then sintered in a closed Al 2 0 3 crucible inside a furnace. A temperature of 1 100°C, 1 125°C and 1 150°C, a soaking time of 1 h and heating/cooling rates of ⁇ 3 °C min "1 were selected.
  • Samples for phase and microstructural characterizations were prepared by thinning of ceramics to remove one surface (-100 ⁇ ), followed by polishing to a mirror finish. A final thermal treatment at 600°C for 2h with ⁇ 0.5 °C min "1 was carried out to remove the damage introduced, and to restore the equilibrium polymorphic phase coexistence and domain configurations, which are modified by the shear stresses involved in polishing.
  • XRD X-ray diffraction
  • Microstructure was studied with a FEI NovaTM NanoSEM 230 field emission gun scanning electron microscope equipped with an Oxford INCA 250 electron dispersive X-ray spectrometer for chemical analysis.
  • Ceramic capacitor for electrical and electromechanical characterizations were prepared by thinning discs down 0.5 mm, painting of Ag electrodes on the major faces, and their sintering at 700 °C.
  • Room temperature ferroelectric hysteresis loops were recorded under voltage sine waves of increasing amplitude up to 10 kV with a 0.1 Hz frequency, obtained by the combination of a synthesizer/function generator (HP 3325B) and a high voltage amplifier (TREK model 10/40), while charge was measured with a homebuilt charge to voltage converter and software for loop acquisition and analysis. Subsequently, the ceramic discs were poled for electromechanical characterization. A field of 4 kV mm "1 was applied at 100 °C for 15 min, and maintained during cooling down to 40 °C. The longitudinal piezoelectric coefficient d 33 was then measured 24 h after the poling step with a Berlincourt type meter.
  • the transverse piezoelectric coefficient d 31 was obtained by complex analysis of piezoelectric radial resonances of the discs by an automatic iterative method described in C. Alemany et al J Phys D: Appl Phys 1995; 28:945. This procedure also provides the Sn E and s i2 E compliances and ⁇ 33 ⁇ permittivity of the poled material all in complex form and thus, all mechanical, electrical and electromechanical losses.
  • magnetoelectric composites were fabricated with selected Bi 1 -x+ 2yPb x-3y Sci- x Ti x 0 3 compositions.
  • Three-layer structures consisting of one piezoelectric ceramic disc, glued between two Terfenol-D metal alloy pieces (ETREMA Products Inc.) by using a silver loaded epoxy adhesive were built, and their magnetoelectric response characterized.
  • a system comprising a combination of two Helmholtz coils, designed to independently provide a static magnetic field up to 1 kOe to magnetize the material, and an alternate magnetic field up to 10 Oe at 10 kHz to play as stimulus (Serviciencia S.L.), was used, while the magnetoelectric voltage response was monitored with a lock-in amplifier.
  • a 31 geometry was chosen to obtain the transverse magnetoelectric coefficient a 31 as a function of the bias magnetic field H, after normalization to the piezoelectric element thickness (0.5 mm).
  • Microstructure coarsening was also targeted, so sintering experiments at 1 125 and 1 150°C were additionally carried out.
  • a first result worth commenting on is the very large enhancement of permittivity experienced by the materials at the core of the MPB after poling.
  • this enhancement is basically a consequence of the reduced permittivity of the poled material, and it is not caused by a decrease of the domain wall contribution, but of the single crystal one, either as a consequence of the modification of the phase coexistence or a direct effect of the presence of the point defects in polarizability.
  • the material has also a strongly decreased elastic compliance; one can assume then that the incorporation of the point defects causes an overall increase of the lattice rigidity with a direct effect on polarizability and deformability.
  • a new application of high sensitivity piezoelectrics is magnetoelectric composites, in which they are combined with magnetostrictive materials to provide magnetoelectricity as a product property. Magnetoelectric transducers are being considered for a range of technologies like high sensitivity, room temperature operation magnetic field sensors. It has been shown that the voltage magnetoelectric coefficient of the simplest two-layer piezoelectric-magnetostrictive structure is given by

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

L'invention concerne un matériau céramique BiScO3-PbTiO3 piézoélectrique à haute température ayant pour formule Bi1-x+2yPbx-3ySc1-xTixO3, avec x compris dans la plage de 0,64 à 0,68 et y compris dans la plage de 0,01 à 0,025, lequel comprend un défaut ponctuel conçu pour améliorer la réponse en tension. L'invention concerne en outre un procédé pour obtenir ledit matériau céramique par frittage conventionnel de poudres nanocristallines synthétisées par activation mécanochimique d'un mélange stœchiométrique de précurseurs. Pour terminer, l'invention concerne également l'utilisation du matériau céramique BiScO3-PbTiO3 modifié chimiquement en tant que partie de dispositifs de détection et de dispositifs de détection magnétique.
PCT/EP2016/082337 2015-12-29 2016-12-22 Matériau céramique bisco3-pbtio3 piézoélectrique à haute température chimiquement modifié pour une réponse en tension améliorée, et procédé pour obtenir ledit matériau céramique Ceased WO2017114741A1 (fr)

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ES201531920A ES2620690B1 (es) 2015-12-29 2015-12-29 UN MATERIAL CERÁMICO PIEZOELÉCTRICO DE ALTA TEMPERATURA DE BiScO3-PbTiO3 DISEÑADO QUÍMICAMENTE PARA POTENCIAR LA RESPUESTA EN VOLTAJE Y PROCEDIMIENTO PARA OBTENER DICHO MATERIAL CERÁMICO

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108470824A (zh) * 2018-03-15 2018-08-31 南方科技大学 一种耐高温的多层压电陶瓷致动器及其制备方法和用途
EP3409652A1 (fr) * 2017-05-31 2018-12-05 Consejo Superior de Investigaciones Cientificas (CSIC) Température élevée et tension piézo-électrique de réponse, matériau céramique à base de bisco3-pbtio3 microstructurellement conçu pour une meilleure performance mécanique, procédure permettant d'obtenir ledit matériau céramique et son utilisation comme dispositif de détection
EP3409651A1 (fr) * 2017-05-31 2018-12-05 Consejo Superior de Investigaciones Cientificas (CSIC) Matériau céramique à base de bisco3-pbtio3 piézoélectrique et à haute température, microstructurellement conçu pour une meilleure performance mécanique, procédure permettant d'obtenir ledit matériau céramique et son utilisation en tant que partie d'un dispositif de génération d'ultrasons ou d'un dispositif d'actionnement par ultrasons
CN109596209A (zh) * 2018-12-07 2019-04-09 苏州长风航空电子有限公司 一种高温压电振动传感器及压电元件制备方法
CN111170736A (zh) * 2020-02-26 2020-05-19 中国科学院上海硅酸盐研究所 一种铅基钙钛矿结构高温压电陶瓷及其制备方法
CN116063071A (zh) * 2023-01-16 2023-05-05 西安电子科技大学 一种高温压电陶瓷材料及其相界调控方法

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CN115385683B (zh) * 2022-08-29 2023-07-25 西安交通大学 一种兼具高居里温度和高压电系数的压电陶瓷材料及其制备方法

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CHEN Y ET AL: "Bismuth-modified BiScO"3-PbTiO"3 piezoelectric ceramics with high Curie temperature", MATERIALS LETTERS, ELSEVIER, AMSTERDAM, NL, vol. 62, no. 20, 31 July 2008 (2008-07-31), pages 3567 - 3569, XP022695519, ISSN: 0167-577X, [retrieved on 20080404], DOI: 10.1016/J.MATLET.2008.03.056 *
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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3409652A1 (fr) * 2017-05-31 2018-12-05 Consejo Superior de Investigaciones Cientificas (CSIC) Température élevée et tension piézo-électrique de réponse, matériau céramique à base de bisco3-pbtio3 microstructurellement conçu pour une meilleure performance mécanique, procédure permettant d'obtenir ledit matériau céramique et son utilisation comme dispositif de détection
EP3409651A1 (fr) * 2017-05-31 2018-12-05 Consejo Superior de Investigaciones Cientificas (CSIC) Matériau céramique à base de bisco3-pbtio3 piézoélectrique et à haute température, microstructurellement conçu pour une meilleure performance mécanique, procédure permettant d'obtenir ledit matériau céramique et son utilisation en tant que partie d'un dispositif de génération d'ultrasons ou d'un dispositif d'actionnement par ultrasons
CN108470824A (zh) * 2018-03-15 2018-08-31 南方科技大学 一种耐高温的多层压电陶瓷致动器及其制备方法和用途
CN109596209A (zh) * 2018-12-07 2019-04-09 苏州长风航空电子有限公司 一种高温压电振动传感器及压电元件制备方法
CN111170736A (zh) * 2020-02-26 2020-05-19 中国科学院上海硅酸盐研究所 一种铅基钙钛矿结构高温压电陶瓷及其制备方法
CN111170736B (zh) * 2020-02-26 2021-04-16 中国科学院上海硅酸盐研究所 一种铅基钙钛矿结构高温压电陶瓷及其制备方法
CN116063071A (zh) * 2023-01-16 2023-05-05 西安电子科技大学 一种高温压电陶瓷材料及其相界调控方法

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