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

Anew heterometal-pseudo-Alkoxide, [(bpy)Cl₂Pb(μ-O^tBu)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 tertbutoxy 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 byTGA analysis (equation (1)). [pby]Cl₂Pb(μ- O^tBu)₂ZrCl₂(THF)2 1st Step T=367 °C-42.67% Cl₂Pb(O)₄ZrCl₂ × 2nd Step → T=804 °C-35.67% ZrO₂ 3rd Step → T=>1000 °C>-4.86% Pure ZrO₂ 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, EDXand IR spectroscopy, were used to find the composition, phase, and morphology of the resulting powder. The post sintering (400 °C) sample was confirmed as ZrO₂Pb₃O₄ 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.