Synthesis of nano-bound microsphere Co3O4 by simple polymer-assisted sol–gel technique

Abstract

Nano-bound Co3O4 microspheres and molten Co3O4 microspheres were synthesized for the first time by a simple polymer (poly-(vinylpyrrolidone))-assisted sol–gel and sol–gel technique, respectively. Thermal decomposition of the precursor samples of both polymer-assisted sol–gel and sol–gel technique were studied by thermogravimetric analysis. In both techniques, the material was calcined at different temperatures for the formation of phase pure Co3O4. X-ray diffraction confirmed the formation of phase pure cubic spinel structured Co3O4 at 400 and 500 °C for the polymer-assisted sol–gel and sol–gel technique, respectively. Fourier transform infrared spectroscopy revealed the vibrational assignments of functional groups associated with the cubic spinel structure of Co3O4. Scanning electron microscopy of all samples showed clear microsphere sizes ranging from 1 to 4 μm. Both techniques allowed the formation of spherical-shaped microspheres by a simple process. Nano-bound microspheres were observed from the polymer-assisted sol–gel technique because the decomposition of PVP at 400 °C is the main reason for the formation of nano-bound microspheres. The nanoparticle size of the nano-bound microsphere measured by transmission electron microscopy was ~40 nm. Therefore, PVP is an essential compound for the formation of nano-bound microspheres. This very simple and inexpensive technique is suitable for the formation of spherical-shaped microspheres.