caa a22 4500 463231953 CHVBK 20180405153245.0 cr unu---uuuuu 170326e20070101xx s 000 0 eng 10.1007/s10853-006-1154-9 doi (NATIONALLICENCE)springer-10.1007/s10853-006-1154-9 The aqueous solution-gel synthesis of perovskite Pb(Zr1−x,Tix)O3 (PZT) [Elektronische Daten] [K. Van Werde, G. Vanhoyland, D. Mondelaers, H. Den Rul, M. Van Bael, J. Mullens, L. Van Poucke] Starting from a novel water-based Zr(IV)-peroxo-citrato solution, an entirely aqueous solution-gel synthesis of Pb(Zr0.53,Ti0.47)O3 (PZT) was carried out. Because of the tendency of Zr4+-ions to hydrolyze and condensate extensively in water, the Zr4+-ions had to be chemically modified by reaction with hydrogen peroxide and citric acid in a two-step precursor synthesis. A transparent amorphous PZT gel precursor was obtained by evaporating the solvent (water). This resulted in a network of cross-linked ammonium-carboxylate bonds that holds Zr(IV)-peroxo-citrato, Ti(IV)-peroxo-citrato and Pb(II)-citrate complexes. By combining complementary thermal analysis techniques such as HT-DRIFT (high-temperature diffuse reflectance Fourier-transform infrared spectroscopy), TGA-MS (thermogravimetrical analysis online coupled to mass spectrometry) and DTA (differential thermal analysis) insight in the decomposition mechanism of the PZT gel was gained. Three major regions could be distinguished; consecutively the non-coordinative matrix surrounding the metal ion complexes, the precursor complexes and the remaining organic matrix are being decomposed. The phase formation of crystalline perovskite PZT was investigated in situ by means of HT-XRD (high-temperature X-ray diffraction). It shows that sublimation of PbO leads to the phase segregation of a Zr-rich PZT phase when a stoichiometric PZT precursor is used. Single phase perovskite PZT however can be obtained at low temperature (∼610°C) when a 16 % lead excess is applied. Springer Science+Business Media, LLC, 2006 Van Werde K. Laboratory of Inorganic and Physical Chemistry, IMO, Limburgs Universitair Centrum, B-3590, Diepenbeek, Belgium aut Vanhoyland G. Laboratory of Inorganic and Physical Chemistry, IMO, Limburgs Universitair Centrum, B-3590, Diepenbeek, Belgium aut Mondelaers D. Laboratory of Inorganic and Physical Chemistry, IMO, Limburgs Universitair Centrum, B-3590, Diepenbeek, Belgium aut Den Rul H. Laboratory of Inorganic and Physical Chemistry, IMO, Limburgs Universitair Centrum, B-3590, Diepenbeek, Belgium aut Van Bael M. Laboratory of Inorganic and Physical Chemistry, IMO, Limburgs Universitair Centrum, B-3590, Diepenbeek, Belgium aut Mullens J. Laboratory of Inorganic and Physical Chemistry, IMO, Limburgs Universitair Centrum, B-3590, Diepenbeek, Belgium aut Van Poucke L. Laboratory of Inorganic and Physical Chemistry, IMO, Limburgs Universitair Centrum, B-3590, Diepenbeek, Belgium aut Journal of Materials Science Kluwer Academic Publishers-Plenum Publishers; http://www.springer-ny.com 42/2(2007-01-01), 624-632 0022-2461 42:2<624 2007 42 10853 https://doi.org/10.1007/s10853-006-1154-9 text/html Onlinezugriff via DOI 1 research-article jats NATIONALLICENCE 856 40 https://doi.org/10.1007/s10853-006-1154-9 text/html Onlinezugriff via DOI NATIONALLICENCE 700 1- Van Werde K. Laboratory of Inorganic and Physical Chemistry, IMO, Limburgs Universitair Centrum, B-3590, Diepenbeek, Belgium aut NATIONALLICENCE 700 1- Vanhoyland G. Laboratory of Inorganic and Physical Chemistry, IMO, Limburgs Universitair Centrum, B-3590, Diepenbeek, Belgium aut NATIONALLICENCE 700 1- Mondelaers D. Laboratory of Inorganic and Physical Chemistry, IMO, Limburgs Universitair Centrum, B-3590, Diepenbeek, Belgium aut NATIONALLICENCE 700 1- Den Rul H. Laboratory of Inorganic and Physical Chemistry, IMO, Limburgs Universitair Centrum, B-3590, Diepenbeek, Belgium aut NATIONALLICENCE 700 1- Van Bael M. Laboratory of Inorganic and Physical Chemistry, IMO, Limburgs Universitair Centrum, B-3590, Diepenbeek, Belgium aut NATIONALLICENCE 700 1- Mullens J. Laboratory of Inorganic and Physical Chemistry, IMO, Limburgs Universitair Centrum, B-3590, Diepenbeek, Belgium aut NATIONALLICENCE 700 1- Van Poucke L. Laboratory of Inorganic and Physical Chemistry, IMO, Limburgs Universitair Centrum, B-3590, Diepenbeek, Belgium aut NATIONALLICENCE 773 0- Journal of Materials Science Kluwer Academic Publishers-Plenum Publishers; http://www.springer-ny.com 42/2(2007-01-01), 624-632 0022-2461 42:2<624 2007 42 10853 Metadata rights reserved Springer special CC-BY-NC licence nationallicence BK010053 XK010053 XK010000 NATIONALLICENCE NATIONALLICENCE NL-springer