A new single source molecular precursor for synthesis of ZrO2/Pb3O4 nanocomposite by co-precipitation enhanced sol—gel method

Abstract

A new heterometal-pseudo-alkoxide, [(bpy)Cl2Pb(μ-OtBu)2ZrCl2(THF)2], compound was developed, and applied as single source molecular precursor (SSP) for the synthesis of ZrO2/Pb3O4 nanocomposite employing co-precipitation enhanced sol–gel method. The SSP has been obtained in the form of monomer in which the metallic centers are bridged through the oxygen atom of the tert-butoxy group. The bipyridyl (bpy) and tetrahydroduran (THF), respectively, coordinated to the lead (Pb) and zirconium (Zr) centers contain the degree of polymerization of the bimetallic molecule. The chlorides present as terminal groups are balancing the overall charge of the molecule. The thermal decomposition pattern of the SSP was established by TGA analysis (equation (1)).1 pby Cl 2 Pb &mgr; − O t Bu 2 ZrCl 2 THF 2 ⟶ T = 367 ° C − 42.67 % 1 st Step Cl 2 Pb O 4 ZrCl 2 × ⟶ T = 804 ° C − 35.67 % 2 nd Step ZrO 2 ⟶ T = > 1000 ° C > − 4.86 % 3 rd Step Pure ZrO 2 ?>The molecular SSP was hydrolyzed by adding an equimolar amount of water and the powder was precipitated at pH = 10 adding NH4OH solution as co-precipitating agent. The analytical techniques, i.e. XRD, SEM, EDX and IR spectroscopy, were used to find the composition, phase, and morphology of the resulting powder. The post sintering (400 °C) sample was confirmed as ZrO2/Pb3O4 nanocomposite. However, the pre-sintering material was amorphous. The pre- and post-sintering samples have rod-shaped nanoparticles. The latter have thinner nanorods than the former.