WO2015018915A1 - Piezokeramischer werkstoff mit reduziertem bleigehalt - Google Patents

Piezokeramischer werkstoff mit reduziertem bleigehalt Download PDF

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Publication number
WO2015018915A1
WO2015018915A1 PCT/EP2014/067036 EP2014067036W WO2015018915A1 WO 2015018915 A1 WO2015018915 A1 WO 2015018915A1 EP 2014067036 W EP2014067036 W EP 2014067036W WO 2015018915 A1 WO2015018915 A1 WO 2015018915A1
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Prior art keywords
piezoceramic material
piezoceramic
mixture
material according
addition
Prior art date
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Ceased
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PCT/EP2014/067036
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German (de)
English (en)
French (fr)
Inventor
Eberhard Hennig
Antje Kynast
Michael TÖPFER
Michael Hofmann
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PI Ceramic GmbH Keramische Technologien und Bauelemente
Original Assignee
PI Ceramic GmbH Keramische Technologien und Bauelemente
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Filing date
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Application filed by PI Ceramic GmbH Keramische Technologien und Bauelemente filed Critical PI Ceramic GmbH Keramische Technologien und Bauelemente
Priority to EP14750209.0A priority Critical patent/EP3030537B1/de
Priority to CN201480050911.3A priority patent/CN105555736B/zh
Priority to US14/909,786 priority patent/US10910550B2/en
Priority to DK14750209.0T priority patent/DK3030537T5/en
Priority to JP2016532695A priority patent/JP2016528151A/ja
Publication of WO2015018915A1 publication Critical patent/WO2015018915A1/de
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • 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
    • C04B35/495—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 vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
    • C04B35/62655—Drying, e.g. freeze-drying, spray-drying, microwave or supercritical drying
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/62695—Granulation or pelletising
    • 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
    • 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
    • H10N30/8542—Alkali metal based oxides, e.g. lithium, sodium or potassium niobates
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    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3251—Niobium oxides, niobates, tantalum oxides, tantalates, or oxide-forming salts thereof
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    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3262—Manganese oxides, manganates, rhenium oxides or oxide-forming salts thereof, e.g. MnO
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    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3294—Antimony oxides, antimonates, antimonites or oxide forming salts thereof, indium antimonate
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    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3296—Lead oxides, plumbates or oxide forming salts thereof, e.g. silver plumbate
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    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
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    • C04B2235/79—Non-stoichiometric products, e.g. perovskites (ABO3) with an A/B-ratio other than 1

Definitions

  • the invention relates to a piezoceramic material with a reduced lead content based on potassium sodium niobate (KNN) based on a basic composition according to the preamble of claim 1.
  • KNN potassium sodium niobate
  • PZT lead zirconate titanate
  • KNN potassium sodium niobate
  • EP1382588A1 describes a lead-free piezoceramic
  • Composition having a main component of the general formula ⁇ Li x (Ki-yNay) i- x ⁇ (Nbi- z z -wTa Sbw) 03 and at least one metallic element selected from (1) palladium, silver, gold, ruthenium, rhodium, rhenium , Osmium, iridium and platinum or (2) nickel, iron, manganese, copper, zinc or (3) magnesium, calcium, strontium and barium as an additional element.
  • metallic element selected from (1) palladium, silver, gold, ruthenium, rhodium, rhenium , Osmium, iridium and platinum or (2) nickel, iron, manganese, copper, zinc or (3) magnesium, calcium, strontium and barium as an additional element.
  • An element comprising a plurality of lead-free piezoelectric layers containing an oxide comprising an alkali metal element, in particular in the form of
  • Sodium, potassium or lithium and contains niobium or bismuth Sodium, potassium or lithium and contains niobium or bismuth.
  • EP2104152A2 describes a piezoelectric element containing a lead-free piezoelectric ceramic.
  • the components KNb0 3 and BaTi0 3 are called.
  • Piezoelectric ceramics have the general formula xKNb0 3 - (lx) BaTi0 3 , where x is between 0.5 and 0.9.
  • EP1876155A1, EP1876156A1 and DE112006003755B4 are directed to a
  • EP 1702906A1 describes a piezoceramic material in which a basic ceramic composition is prepared by adding, for example,
  • Alkaline earth metal metaniobate is modified.
  • KNN potassium natrium mN iobate
  • a piezoelectric multilayer actuator based on a material according to the invention is defined as defined in claim 13.
  • the use of a mixture of Pb, Nb and optiona Ag in is also suitable a piezoceramic material of potassium niobium niobate (KNN) base to increase the sintering interval. It is therefore from a lead-free piezoceramic material on potassium sodium niobate (KNN) basis of the basic composition
  • the data k, I and m refer to the wt .-% of the respective component based on the total mass of the piezoceramic
  • Nb can be wholly or partially replaced by one or more of the elements Ta and Sb.
  • the piezoceramic material according to the invention thus has the
  • Basic composition contains a further component comprising Pb, Nb and optionally Ag, wherein the weight proportions of Pb, Nb and Ag based on the total weight of the piezoceramic material are selected as follows: k wt% Pb + I wt% Nb + m wt% Ag
  • the amount of added Pb is chosen such that 0.001 ⁇ k ⁇ 0.2.
  • Nb is chosen so that 0 ⁇ I ⁇ 0.179.
  • the amounts of Pb and Nb added are chosen to be 0.001 ⁇ k ⁇ 0.11 and 0.022 ⁇ 1 ⁇ 0.09.
  • Component in addition to Pb and Nb and optionally Ag additionally includes Mn.
  • Materials have a sintering interval in the range of> 20 K, in particular in the range of 30 K to 40 K.
  • the reduced lead content piezoceramic material is accomplished through the steps of preparing a calcine of the base composition and adding the sintering aid mixture.
  • the addition of the sintering aid mixture which comprises Pb, Nb and optionally Ag and optionally Mn, can be carried out in particular during fine grinding.
  • the further processing is realized in a known manner including sintering in a normal atmosphere.
  • the invention thus also relates to a method for producing a piezoceramic material with a reduced lead content
  • piezoceramic multilayer actuator on the basis of the piezoceramic material according to the teaching of claim 13.
  • the invention also relates to the use of a mixture of Pb, Nb and optionally Ag in a piezoceramic material to potassium-sodium
  • the amount of added Pb is chosen such that 0.001 ⁇ k ⁇ 0.2.
  • Nb is chosen so that 0 ⁇ I ⁇ 0.179.
  • the amounts of Pb and Nb added are chosen to be 0.001 ⁇ k ⁇ 0.11 and 0.022 ⁇ 1 ⁇ 0.09.
  • Component in addition to Pb and Nb and optionally Ag additionally includes Mn.
  • the ratio of Pb to Mn to Nb prefferably be such that k: b: I is 1: 0.09: 0.30.
  • Bleimetaniobat carried out, wherein the added amount of the sintering aid is selected so that the lead content in the range of 0.05 wt .-% to 0.2 wt .-% is. Particularly preferably, the lead content is at most 0.1 wt .-%, based on the entire piezoceramic material.
  • Fig. 1 describes the general technological process of
  • FIG. 3 shows a comparison of the typical temperature dependence of the specific insulation resistance of exemplary embodiments 1 (prior art) and FIG. 8.
  • FIG. 4a shows the unipolar strain hysteresis
  • FIG. 5a shows the unipolar strain hysteresis
  • FIG. 6a shows the unipolar strain hysteresis
  • Table 1 summarizes the parameters used for the assessment.
  • the specific insulation resistance p is determined at 50V on polarized samples with temperature increase from room temperature to 150 ° C.
  • the electromechanical strain S 3 is determined by laser interferometer at 2kV / mm. For samples that could not be measured at 2 kV / mm due to increased conductivity, the field strength is shown in column 12.
  • Sintering interval is to be understood as the range defined by two temperature specifications, within which the required properties of the ceramic are achieved when the material is fired. These are defined as follows:
  • This composition corresponds to the prior art with a sintering interval ⁇ 20K.
  • Embodiment 2 is a diagrammatic representation of Embodiment 1:
  • This composition according to the invention has a widening of the sintering interval to 30K.
  • This composition according to the invention has a widening of the sintering interval to 30K.
  • This composition according to the invention has a widening of the sintering interval to 30K.
  • Embodiment 5 is a diagrammatic representation of Embodiment 5:
  • This composition according to the invention has a widening of the sintering interval to 30K.
  • Embodiment 6 is a diagrammatic representation of Embodiment 6
  • Embodiment 7 is a diagrammatic representation of Embodiment 7:
  • This composition has a
  • Embodiment 8 is a diagrammatic representation of Embodiment 8
  • This inventive composition has a widening of the sintering interval to 40K.
  • a large-scale processing of the material was carried out throughout and the addition of Pb and Nb during spray granulation.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Compositions Of Oxide Ceramics (AREA)
PCT/EP2014/067036 2013-08-07 2014-08-07 Piezokeramischer werkstoff mit reduziertem bleigehalt Ceased WO2015018915A1 (de)

Priority Applications (5)

Application Number Priority Date Filing Date Title
EP14750209.0A EP3030537B1 (de) 2013-08-07 2014-08-07 Piezokeramischer werkstoff mit reduziertem bleigehalt
CN201480050911.3A CN105555736B (zh) 2013-08-07 2014-08-07 具有减少的铅含量的压电陶瓷材料
US14/909,786 US10910550B2 (en) 2013-08-07 2014-08-07 Piezoceramic material with reduced lead content
DK14750209.0T DK3030537T5 (en) 2013-08-07 2014-08-07 Piezoceramic material with reduced lead content
JP2016532695A JP2016528151A (ja) 2013-08-07 2014-08-07 鉛含有量が低減された圧電セラミック材料

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
DE102013013182.0 2013-08-07
DE102013013182 2013-08-07
DE102014111285.7A DE102014111285A1 (de) 2013-08-07 2014-08-07 Piezokeramischer Werkstoff mit reduziertem Bleigehalt
DE102014111285.7 2014-08-07

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Publication Number Publication Date
WO2015018915A1 true WO2015018915A1 (de) 2015-02-12

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US (1) US10910550B2 (enExample)
EP (1) EP3030537B1 (enExample)
JP (2) JP2016528151A (enExample)
CN (1) CN105555736B (enExample)
DE (1) DE102014111285A1 (enExample)
DK (1) DK3030537T5 (enExample)
WO (1) WO2015018915A1 (enExample)

Cited By (1)

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Publication number Priority date Publication date Assignee Title
JP2018082015A (ja) * 2016-11-15 2018-05-24 セイコーエプソン株式会社 圧電素子、圧電素子応用デバイス及び圧電素子の製造方法

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WO2015179227A1 (en) 2014-05-18 2015-11-26 Children's Medical Center Corporation Methods and compositions relating to exosomes
CN107008636B (zh) * 2017-05-11 2019-08-16 上海师范大学 一种无铅压电单晶高频超声换能器及其制备方法
WO2025229939A1 (ja) * 2024-04-30 2025-11-06 京セラ株式会社 圧電磁器および圧電素子

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Publication number Priority date Publication date Assignee Title
DE10234787C1 (de) 2002-06-07 2003-10-30 Pi Ceramic Gmbh Keramische Tec Verfahren zur Herstellung eines monolithischen Vielschichtaktors, monolithischer Vielschichtaktor aus einem piezokeramischen oder elektrostriktiven Material
EP1382588A1 (en) 2002-07-16 2004-01-21 Denso Corporation Piezoelectric ceramic composition and method of production of same, piezoelectric element, and dielectric element
EP1702906A1 (en) 2003-12-22 2006-09-20 TDK Corporation Piezoelectric porcelain and method for production thereof
DE102007013874A1 (de) 2006-03-20 2007-10-04 Tdk Corp. Mehrschichtiges piezoelektrisches Element
EP1876156A1 (en) 2005-04-28 2008-01-09 Murata Manufacturing Co., Ltd. Piezoelectric ceramic composition, process for producing said piezoelectric ceramic composition, and piezoelectric ceramic electronic component
EP1876155A1 (en) 2005-04-28 2008-01-09 Murata Manufacturing Co., Ltd. Piezoelectric porcelain composition and piezoelectric ceramic electronic component
EP2104152A2 (en) 2008-03-19 2009-09-23 TDK Corporation Piezoelectric ceramic and piezoelectric element employing it
DE112006003755B4 (de) 2006-02-17 2011-06-01 Murata Mfg. Co., Ltd., Nagaokakyo-shi Piezoelektrische Keramikzusammensetzung
DE102010041567A1 (de) * 2010-09-28 2012-03-29 Siemens Aktiengesellschaft Bleifreier, texturierter piezokeramischer Werkstoff mit Haupt- und Nebenphase und anisometrischen Keimen, Verfahren zum Herstellen eines piezokeramischen Bauteils mit dem Werkstoff und Verwendung dazu

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