In this work, Cobalt oxide nanoparticles (Co3O4·NPs) were synthesized via a simple sonochemical reaction by using polyethylene glycol (PEG) as a surfactant. Structural, morphological and spectroscopic analysis of obtained powder (Co3O4·NPs) was investigated by X-ray diffraction, FTIR spectroscopy and scanning electron microscope (SEM). The nanocrystalline nature of the sample was confirmed by XRD, which exhibits the cubic face-centered normal spinel structure of (Co3O4·NPs) and the space group of Fd-3m with the average crystallite size around 15 nm. FTIR spectrum shows two strong absorption bands of (Co+2–O) and (Co+3–O) which confirm the spinel structure of Co3O4·NPs. Moreover, SEM micrographs showed that the agglomeration of the nanoparticles was reduced by the addition of (PEG) surfactant and UV-Vis was used to study the synthesized material’s optical properties. The Co3O4 band gap ranged around 2.2 and 3.5 eV.