Copper oxide and cobalt oxide (CuO, Co3O4) nanocrystals (NCs) have been successfully prepared in a short time using microwave irradiation without any postannealing treatment. Both kinds of nanocrystals (NCs) have been prepared using copper nitrate and cobalt nitrate as the starting materials and distilled water as the solvent. The resulted powders of nanocrystals (NCs) were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), and atomic force microscopy (AFM) measurements. The obtained results confirm the presence of the both of oxides nanopowders produced during chemical precipitation using microwave irradiation. A strong emission under UV excitation is obtained from the prepared CuO and Co3O4nanoparticles. The results show that the nanoparticles have high dispersion and narrow size distribution. The line scans of atomic force microscopy (AFM) images of the nanocrystals (NCs) sprayed on GaAs substrates confirm the results of both X-ray diffraction and transmission electron microscopy. Furthermore, vibrational studies have been carried out using Raman spectroscopic technique. Specific Raman peaks have been observed in the CuO and Co3O4nanostructures, and the full width at half maximum (FWHM) of the peaks indicates a small particle size of the nanocrystals.