Chloro-free route to mixed-metal oxides. Synthesis of lead titanate nanoparticles from a single-source precursor route
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A new heterobimetallic nitrilotriacetatoperoxotitanate complex of titanium and lead [Pb(H2O)3]2[Ti2(O2)2O(nta)2]·4H2O (C6H6O6N=H3nta) was isolated in pure crystals directly from the solution containing tetrabutyl orthotitanate, hydrogen peroxoide, lead acetate, and nitrilotriacetic acid at pH = 2.0–4.0. The isolated complex was characterized by elemental analyses, IR spectrum, thermal analysis (TG), and single-crystal X-ray diffraction. The single-crystal X-ray structural analysis revealed that the titanium atom is N,O,O′,O′′-chelated by the nitrilotriacetate and O,O′-chelated by the peroxo group and was coordinated to the bridging O atom in an overall pentagonal-bipyramidal geometry. The thermal decomposition of this precursor led to the formation of phase-pure lead titanate (PbTiO3) at ≥450 °C. The morphology, microstructure, and crystalline of the resulting PbTiO3 product have been characterized by BET, transmission electron microscopy, and powder X-ray diffraction. The TEM micrographs revealed that the size of the as-synthesized crystallines to be 50–100 nm range. The BET measurement revealed that the PbTiO3 powders had a surface area of 5.6 m2/g.
KeywordsSingle-source precursor Lead titanate (PbTiO3) Nitrilotriacetatoperoxotitanate Carboxylate-containing ligands
We thank “The Fundamental Research Funds for the Central Universities, SCUT (No. 2009ZM0313)”. We also thank “The National Science Foundation of China (No. B5080320)” and the “SRP” of South China University of Technology.
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