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Low temperature hydrothermal synthesis and formation mechanisms of lead titanate (PbTiO3) particles using tetramethylammonium hydroxide: thermodynamic modelling and experimental verification

Journal of the European Ceramic Society
Publication Date
DOI: 10.1016/s0955-2219(03)00085-2
  • Actuators
  • Pbtio3
  • Platelets
  • Powders-Chemical Preparation
  • Thermodynamic Modelling
  • Earth Science
  • Geography
  • Physics


Abstract Thermodynamic modeling was used to predict the optimum synthesis conditions for precipitation of the phase-pure lead titanate (PbTiO 3) in the Pb–Ti-tetramethylammonium hydroxide (TMAH) system using a newly developed computer program for automatic generation of stability and yield diagrams. The thermodynamic model has been experimentally validated over a wide range of processing conditions. Like KOH-mineralized systems, it was determined that the pH of the hydrothermal reaction medium and the Pb/Ti ratio are critical factors in forming stoichiometric PbTiO 3 powder. Morphological evolution during the reaction suggests that the formation mechanism appears to be controlled by a dissolution and recrystallization process. Two possible growth mechanisms are proposed based on the magnitude of the Pb/Ti ratio. In the case of Pb/Ti ratio=1.1, at the early stage of the reaction (3 h) excess lead species promote the formation of spherical intermediate pyrochlore phase followed by the formation of primary cubic PbTiO 3 crystals. The growth of cubic PbTiO 3 crystals proceeds until the intermediate phase acting as a reservoir to provide precipitating ions is consumed. In case of Pb/Ti ratio=1.25, excess lead condition leads to the formation of a platelet-shaped intermediate pyrochlore phase. These platelet intermediate particles act as a template in which small cubic shaped PbTiO 3 grains grew on the surface of these platelets.

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