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DOI: 10.1039/A605266E (Paper) Reference Section for: J. Mater. Chem., 1997, 7, 753-762

Solution routes to lead titanate: synthesis, molecular structure and reactivity of the Pb–Ti and Pb–Zr species formed between various lead oxide precursors and titanium or zirconium alkoxides. Molecular structure of Pb2Ti2(µ4 -O)(OAc)2(OPri)8 and of PbZr3(µ4-O)(OAc)2(OPri) 10

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Liliane G. Hubert-Pfalzgraf, Stéphane Daniele, Renée Papiernik, Marie-Cécile Massiani, Bernard Septe, Jacqueline Vaissermann and Jean-Claude Daran

Abstract

The reactions between Ti(OR)4 (R=Et, Pri) or [Zr(OPri)4(PriOH)]2 and various lead oxide precursors [anhydrous Pb(OAc)2 , alkoxides or oxoalkoxides] have been investigated in different experimental conditions (solvent, temperature). Various mixed-metal species have been isolated in high yields and characterized by microanalysis, FTIR and multinuclear NMR (1H, 13C and 207Pb) spectroscopies. The mixed-metal oxoacetatoalkoxides Pb2Ti2(µ4-O)(µ-OAc)2 (µ-OPri)5(OPri)3 1 and PbZr3(µ4-O)(µ-OAc)2 (µ-OPri)5(OPri)5 2 have been characterized by X-ray crystallography at -100 °C: for 1, monoclinic, space group C2 /c with a=38.916(17) Å, b=12.045(2) Å, c=19.046(4) Å, β=112.84(3)°, V=8224(4) Å3 , Z=8, R=0.068, Rw=0.076; and for 2, monoclinic, space group P21 /n with a=10.618(2) Å, b=25.157(11) Å, c=18.611(5) Å, β=90.35(2)°, V=4971(3) Å3 , Z=4, R=0.060, Rw=0.072. Hydrolysis–condensation reactions have been achieved especially for the species having a Pb:Ti stoichiometry appropriate for access to PbTiO3 . Effects of the solvent on the temperature of crystallisation and on the particle size are discussed.

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