Solid state synthesis of micro and nanostructured metal oxides using organometallic-polymers precursors

Abstract

The organometallic derivatives of poly(styrene-co-4vinylpyridine), PS-co-4-PVP, of the general formula: {[CH2CH(C6H5)]0.1[CH2CH(C5H4N·MLn)]0.9}n; MLn =W(CO)5, (1), CpRu(PPh3)2(2), CpFe(dppe) (3), Cp2TiCl (4) and CH3-C5H4-Mn(CO)2(5) were prepared from the respective organometallic and the co-polymer {[CH2CH(C6H5)]0.1[CH2CH(C5H4N]0.9}n. The solid state pyrolysis of these derivatives under air and at 800°C give rise to micro and nanostructured powder metal oxides WO3, RuO2, TiO2, Mn2O3and the iron (III) phosphate (FePO4) in the case of the iron precursor. The pyrolytic products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and energy dispersive X-ray scattering (EDX) and infrared spectroscopy (IR). From the TG (thermal gravimetric) and DSC (differential scanning calorimetry) data a possible mechanism for the formation of the solid nanostructured materials is discussed. The method appears to be a reliable and general way to obtain nanostructured metal oxide in solid-state which could be potentially and easily incorporated in solid-state electronics, catalysts and sensor devices.