Due to a dominant one-dimensional growth rate, nanoparticles of zinc oxide often show a rodlike morphology. As a result, the synthesis of small spherical nanoparticles of undoped ZnO remains challenging. This paper presents two procedures that successfully produce a powder consisting of equiaxed zinc oxide nanoparticles: one using a polyethylene glycol- (PEG-) assisted solvothermal method and the other by calcination of zinc oxalate obtained from a microemulsion-mediated method. In the latter, zinc-substituted aerosol OT (AOT) is used as a surfactant. The samples are characterized by inductively coupled plasma-atomic emission spectroscopy (ICP-AES), thermogravimetric analysis (TGA), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), photon correlation spectroscopy (PCS), and photoluminescence (PL) spectroscopy. Both synthesis techniques produce nanoparticles with similar sizes in the range of 10 to 20 nm. Dense aggregates observed in the calcined powder are infrequent in the case of the solvothermal method.