Chloro-free route to mixed-metal oxides. Synthesis of lead titanate nanoparticles from a single-source precursor route

• Published in: Journal of thermal analysis and calorimetry 2011-05, Vol.104 (2), p.653-659
• Main Authors: Tang, Shidi, Deng, Yuanfu, Zhan, ShuZhong
• Format: Article
• Language: English
• Subjects: Analysis; Analytical Chemistry; Atomic structure; Chemistry; Chemistry and Materials Science; Crystal structure; Diffraction; Exact sciences and technology; Inorganic Chemistry; Inorganic chemistry and origins of life; Lead titanates; Measurement Science and Instrumentation; Miscellaneous; Oxides; Physical Chemistry; Polymer Sciences; Precursors; Preparations and properties; Thermal analysis; Titanium; X-rays
• ISSN: 1388-6150; 1588-2926; 1572-8943
• DOI: 10.1007/s10973-010-0999-y

A new heterobimetallic nitrilotriacetatoperoxotitanate complex of titanium and lead [Pb(H 2 O) 3 ] 2 [Ti 2 (O 2 ) 2 O(nta) 2 ]·4H 2 O (C 6 H 6 O 6 N=H 3 nta) 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 (PbTiO 3 ) at ≥450 °C. The morphology, microstructure, and crystalline of the resulting PbTiO 3 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 PbTiO 3 powders had a surface area of 5.6 m 2 /g.