EP2411347A1 - Bleizirkonattitanate und verfahren zu deren herstellung - Google Patents
Bleizirkonattitanate und verfahren zu deren herstellungInfo
- Publication number
- EP2411347A1 EP2411347A1 EP10710338A EP10710338A EP2411347A1 EP 2411347 A1 EP2411347 A1 EP 2411347A1 EP 10710338 A EP10710338 A EP 10710338A EP 10710338 A EP10710338 A EP 10710338A EP 2411347 A1 EP2411347 A1 EP 2411347A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- lead zirconate
- zirconate titanate
- sintering
- zirconium
- less
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Ceased
Links
- 238000000034 method Methods 0.000 title claims abstract description 32
- 238000004519 manufacturing process Methods 0.000 title abstract description 3
- 229910052451 lead zirconate titanate Inorganic materials 0.000 claims abstract description 54
- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 17
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002245 particle Substances 0.000 claims abstract description 11
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 7
- 150000003755 zirconium compounds Chemical class 0.000 claims abstract description 5
- 238000005245 sintering Methods 0.000 claims description 46
- 239000000919 ceramic Substances 0.000 claims description 30
- 239000000843 powder Substances 0.000 claims description 21
- 230000008569 process Effects 0.000 claims description 16
- 239000010936 titanium Substances 0.000 claims description 9
- 238000001354 calcination Methods 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000013078 crystal Substances 0.000 claims description 4
- 239000007772 electrode material Substances 0.000 claims description 4
- 239000007791 liquid phase Substances 0.000 claims description 4
- 229910052758 niobium Inorganic materials 0.000 claims description 3
- 239000010955 niobium Substances 0.000 claims description 3
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 3
- 229910052709 silver Inorganic materials 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 2
- 229910052745 lead Inorganic materials 0.000 claims description 2
- 238000004377 microelectronic Methods 0.000 claims 3
- -1 compounds zirconium hydroxide Chemical class 0.000 claims 2
- 238000006386 neutralization reaction Methods 0.000 claims 2
- 239000012266 salt solution Substances 0.000 claims 2
- 150000003754 zirconium Chemical class 0.000 claims 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims 1
- KGBUQHGXOAESDX-UHFFFAOYSA-N [Zr].OOO Chemical compound [Zr].OOO KGBUQHGXOAESDX-UHFFFAOYSA-N 0.000 claims 1
- 238000000227 grinding Methods 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- 230000003472 neutralizing effect Effects 0.000 claims 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims 1
- 239000012071 phase Substances 0.000 claims 1
- 239000002244 precipitate Substances 0.000 claims 1
- 239000000047 product Substances 0.000 claims 1
- 239000004332 silver Substances 0.000 claims 1
- 229910001928 zirconium oxide Inorganic materials 0.000 claims 1
- 150000002611 lead compounds Chemical class 0.000 abstract description 3
- HTUMBQDCCIXGCV-UHFFFAOYSA-N lead oxide Chemical compound [O-2].[Pb+2] HTUMBQDCCIXGCV-UHFFFAOYSA-N 0.000 description 17
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 239000000370 acceptor Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 239000010949 copper Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 4
- 239000000376 reactant Substances 0.000 description 4
- GQRVVPRMXSHZRA-UHFFFAOYSA-N titanium zirconium hydrate Chemical compound O.[Ti].[Zr] GQRVVPRMXSHZRA-UHFFFAOYSA-N 0.000 description 4
- 239000002019 doping agent Substances 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 229910052688 Gadolinium Inorganic materials 0.000 description 2
- 229910052779 Neodymium Inorganic materials 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 229910052797 bismuth Inorganic materials 0.000 description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 229910000464 lead oxide Inorganic materials 0.000 description 2
- 244000144972 livestock Species 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229910052712 strontium Inorganic materials 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 229910001316 Ag alloy Inorganic materials 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910021193 La 2 O 3 Inorganic materials 0.000 description 1
- 229910001252 Pd alloy Inorganic materials 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- UOKKBZQGTUWMSJ-UHFFFAOYSA-N [W]=O.[Cu].[Ba] Chemical class [W]=O.[Cu].[Ba] UOKKBZQGTUWMSJ-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000006735 deficit Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
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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
- C04B35/48—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 zirconium or hafnium oxides, zirconates, zircon or hafnates
- C04B35/49—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 zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates
- C04B35/491—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 zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates based on lead zirconates and lead titanates, e.g. PZT
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
- C01G25/006—Compounds containing, besides zirconium, two or more other elements, with the exception of oxygen or hydrogen
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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
- C04B35/62675—Thermal treatment of powders or mixtures thereof other than sintering characterised by the treatment temperature
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- 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
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- H10N30/853—Ceramic compositions
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- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3227—Lanthanum oxide 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
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, 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
- C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
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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 piezoceramic compositions in the form of lead zirconate titanates (PZT), a process for their preparation using titanium dioxide particles and a finely divided zirconium compound and a lead compound. Furthermore, the invention relates to a piezoelectric component which contains a lead zirconate titanate,
- PZT Lead zirconate titanate
- PZT powder is usually made from the raw materials lead oxide, zirconia and titanium dioxide.
- the composition can be given by formula as Pb (Zr x Ti; ⁇ x ) ⁇ 3 with 0 ⁇ x ⁇ l.
- doping elements are usually included (generally about 1-3% in total). Typical dopants are lanthanum, neodymium, strontium, potassium, bismuth, tantalum, chromium, cobalt, manganese, iron, gadolinium and niobium.
- PZT Mischoxidpuiver that are pressed into moldings or processed into coatings or films and then sintered into a ceramic.
- Lead zirconate titanate manganese oxide powders can be prepared by synthesis methods that proceed via solid-state reactions (mixed oxide processes) and by wet-chemical methods (eg sol-gel process, coprecipitation process or spray-reaction process).
- the sinterability or sintering temperature of the powder is not only dependent on the composition, but also on the history of the respective material, ie the degree of activation, the particle size and the particle size distribution, the particle shape and the density of the green body (ie after shaping and before sintering ).
- the corresponding sintering temperatures are about 1100-1250 0 C (oxidic reactants) or ⁇ 1000 ° C ⁇ sol-gel reactants). At temperatures significantly higher than 1000 0 C but merkiiche amounts of lead oxide, which is why precautions to avoid lead loss and thereby disturbing the stoichiometry must be taken evaporate.
- the livestock piezoelectric actuators consist of stacked ferroelectric ceramic layers with a layer thickness of about 10 to 200 microns. Between each ceramic layer is an approximately 1-3 microns thick metal electrode, which serves to control the actuator. These livestock piezoelectric actuators ideally have relatively high Curie temperatures, so that applications at higher temperatures are possible. In addition, they are characterized by high piezoelectric and electromechanical characteristics and fatigue resistance.
- compositions are desired which offer a high sintering activity and thus permit the use of low-melting and inexpensive electrode materials by means of a low sintering temperature of the lead zirconate titanates according to the invention.
- a niobium-containing PZT composition As a low sintering system, a niobium-containing PZT composition is known which often contains a high PbO excess as a sintering aid (WO 2008/068096). Disadvantages of these systems, however, are the interactions that occur with other constituents in the finished component, which leads to a deterioration of the electromechanical properties. For use in multilayer systems, chemical reactions and alloying with the electrode materials (Ag, Ag / Pd, or even Cu) deserve particular mention.
- WO 2006/063784 discloses high sintering activity PZT compositions which allow low process temperatures for the sintering step.
- the disadvantage here is the relatively small particle diameter of the PZT, which degrades the technically usable piezoelectric properties of the ceramic.
- acceptor additives has a favorable effect (WO 03/101946).
- Acceptors such as Fe 3+ replace Zr 4+ in the solid, which is compensated by the creation of oxygen vacancies ⁇ RW Schwartz et al., Piezoelectric and Electro-optic Ceramics, in Ceramic Materials for Electronics, RC Buchanan (ed.), 3rd edition, publisher Marcel Dekker, 2004).
- the voids facilitate the diffusion in the solid during the sintering process and thus cause a stronger grain growth.
- a disadvantage of using the acceptor additives is the limited reorientation of the ferroelectric domains, and thus ceramics so treated exhibit poorly developed hysteresis loops, smaller dielectric constants, higher dielectric loss values.
- Typical applications are limited to so-called “high-power devices”, sonar applications or ultrasonic generators (RW Schwartz et al.).
- the present invention is based on the object to produce finely divided, ⁇ interin, easy to process and economically producible lead zirconate titanates, from which PZT ceramics can be produced which compact well while maintaining or improving the electromechanical properties at low sintering temperatures.
- a process for their preparation using simple titanium-containing substrates is to be provided.
- the object is achieved on the one hand by a process for the preparation of lead zirconates by reaction of finely divided titanium dioxide particles and finely divided zirconium compounds with a lead compound, wherein the composition contains a complex doping with an effective donor content between 0 mo!% And 5 mol%, in particular 0, 1-lmol%, more preferably 0.15 to 0.5 mol%.
- the object is further achieved by the provision of lead zirconate titanates which can be prepared by the processes according to the invention.
- the invention also includes the provision of a piezoelectric component, in particular a PZT multilayer actuator, produced by means of a lead zirconate titanate material according to the invention which has a comparatively high Curie temperature.
- FIG. 1 Dense sintered lead zirconate titanates (PZT): a) PZT based on zirconium titanium hydrate (ZTH) according to the invention b) PZT conventionally prepared according to the prior art.
- PZT Dense sintered lead zirconate titanates
- Figure 2 Occurrence of a liquid phase during sintering for ZTH-based PZT with 4 mol% PbO excess.
- Figure 3 Typical diffractogram of a 600 ° C / 2h calcined PZT powder on ZTH basis.
- Figure 4 Observed sintering densities of inventive PZT at different sintering temperature and different doping.
- Figure 5 Observed sintering densities of inventive PZT and reference PZT (undoped) at different sintering temperature and different doping.
- Figure 8 Dielectric and eiektromechanische characteristics for inventive lead zirconate titanate with eff. Donor content of 0.125%.
- Figure 1 shows the sintering densities of different PZT materials.
- the ZTH-based PZT ceramics show a significant reduction in the sintering temperatures compared to conventionally produced PZT.
- Ceramics made from the materials according to the invention can thereby be produced at lower sintering temperatures.
- ceramics with higher densities can be produced at the same sintering temperatures.
- microstructures of the lead zirconate titanates according to the invention are finer-grained than the microstructures of lead zirconate titanate ceramics produced from the oxides of Pb, Zr and Ti.
- the microstructures of the ceramics of the bisizirconate titanates according to the invention are coarser than in the absence of the complex doping with an effective donor content between 0% and 1%.
- doping compounds e.g. Nd, Sr, La, Nb, Gd, Bi, Ta, Cr, Co, Mn, Ca, Na, K, Cu, Ni or Fe salts or the corresponding oxides are added. It is true that the complex doping must have an effective donor content between 0% and 5%.
- a general description of the dopants is:
- Donator D * 1 , ..., D £; Acceptor: A ⁇ , ..., A ⁇
- n and m correspond to the valences of the donor or acceptor ions and a and / or ⁇ to the individual molar fractions.
- the variables x and y indicate the number of dopants used.
- a PbO excess in the mol% range preferably ⁇ 2mol%, is added according to the invention.
- the PbO excess is thus in a range in which no liquid phase sintering is observed.
- Figure 2 shows a comparison of the sintering rate for two different PbO contents of a ZTH-based PZT ceramic.
- the sintering of the materials produced on the basis of the powders according to the invention into ceramics with sufficient densities can be carried out at a particularly low temperature.
- ceramics with relative densities of "% 98 (sintered in air ⁇ can be produced at a sintering temperature of 900 0 C.
- the sintering of the green body takes place at a temperature of 800-1050 0 C and a hold time of 6 hours in air.
- the samples are in a closed and with PbO-saturated aluminum umoxtd T zuregel to avoid a large PbO Vertustes during the sintering process.
- PbO Alfa AESAR, purity 99.99%
- zirconium titanium hydrate preparation according to WO 2006/063784
- La 2 O 3 doping element, Alfa AESAR, purity 99.95%
- Fe 2 O 3 doping element, Fa.
- the sieved powders are pressed uniaxially into green bodies and subsequently densified in a cold isostatic press.
- the sintering of the green body takes place at a temperature of 800-1050 0 C and a holding time of 6 h in air.
- the samples are in a closed and PbO-saturated Aiuminiumoxid crucible to avoid excessive PbO ⁇ / loss during the sintering process.
- Electromechanical data strain hysteresis, bipolar, unipolar strain
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Abstract
Description
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PCT/EP2010/053941 WO2010108988A1 (de) | 2009-03-25 | 2010-03-25 | Bleizirkonattitanate und verfahren zu deren herstellung |
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JP6144753B2 (ja) | 2012-04-10 | 2017-06-07 | エプコス アクチエンゲゼルシャフトEpcos Ag | セラミック材料およびこのセラミック材料を備えるコンデンサ |
CN112279642B (zh) * | 2020-10-22 | 2022-08-05 | 江西欧迈斯微电子有限公司 | 压电纤维及其制备方法 |
CN112960981B (zh) * | 2021-05-07 | 2022-07-01 | 重庆文理学院 | 一种镧、锡掺杂的锆钛酸铅陶瓷材料的制备方法 |
CN115403375B (zh) * | 2022-08-31 | 2023-07-14 | 山东国瓷功能材料股份有限公司 | 一种锆钛酸铅压电陶瓷材料及其制备方法 |
CN116924796B (zh) * | 2023-08-14 | 2024-05-14 | 昆明理工大学 | 一种abo3型低介电损耗陶瓷及其制备方法 |
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DE10393064D2 (de) | 2002-05-29 | 2005-05-19 | Siemens Ag | Piezokeramische Zusammensetzung, Piezokeramischer Körper mit der Zusammensetzung und Verfahren zum Herstellen der Zusammensetzung und des Körpers |
JP2004002069A (ja) * | 2002-05-30 | 2004-01-08 | Tdk Corp | 圧電磁器の製造方法および圧電素子の製造方法 |
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DE102006057691A1 (de) | 2006-12-07 | 2008-06-12 | Robert Bosch Gmbh | Niedrig sinterndes, piezoelektrisches Material auf Blei-Zirkonat-Titanat-Mischkristall-Basis, Verfahren zu dessen Herstellung sowie ein dieses Material umfassendes piezoelektrisches Bauelement |
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Non-Patent Citations (3)
Title |
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"Piezoelectric Ceramics", 1 January 1971, ISBN: 978-0-12-379550-2, article BERNARD JAFFE: "Piezoelectric Ceramics", pages: 154 - 160, XP055544108 * |
NIALL J. DONNELLY ET AL: "Addition of a Sr, K, Nb (SKN) Combination to PZT(53/47) for High Strain Applications", JOURNAL OF THE AMERICAN CERAMIC SOCIETY., vol. 90, no. 2, 12 January 2007 (2007-01-12), US, pages 490 - 495, XP055543653, ISSN: 0002-7820, DOI: 10.1111/j.1551-2916.2006.01450.x * |
See also references of WO2010108988A1 * |
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