Purity and properties of spherical shaped Co3O4 nanocrystals prepared by a polyol route using a domestic microwave oven

Abstract

Obtaining spherical shaped Co3O4 nanocrystals/nanoparticles (considered to be a very promising functional material) at low-cost with chemical purity, reduced crystallite size and useful physicochemical properties has been considered to be challenging. The present work (an attempt in this direction) involves the preparation of spherical shaped Co3O4 nanocrystals from cobalt acetate (dissolved in ethylene glycol) by a polyol synthesis route using a domestic microwave oven along with calcination at a suitable temperature (100/200/300/400 °C used to understand the phase evolution). X-ray diffraction (XRD, including Rietveld), infrared spectral, Raman spectral, energy dispersive X-ray absorption spectral and electron microscopic (SEM/TEM, including SAED) analyses have shown good crystallinity, chemical phase purity, spherical shape, reduced crystallite/particle size and narrow size distribution for the Co3O4 nanocrystal sample calcined at 400 °C. UV-Vis-NIR spectral analysis has shown the existence of multiple bandgap energies (1.51–1.98, 2.44–2.61 and 2.81–3.43 eV). Magnetic measurements have confirmed the antiferromagnetic nature possessing considerable magnetization below and above Neel temperature (TN), which indicates the presence of weak ferromagnetic ordering. The crystallite/particle sizes obtained for the sample calcined at 400 °C through XRD analysis, TEM analysis and using TN value (37.3 K) are 32.0, 33.6 and 31.3 nm, respectively. The method of preparation used is highly yielding, low-cost and more advantageous than many other methods used in the past.