Calcium oxide (CaO) is an important inorganic compound, which is used across various industries as catalyst, toxic-waste remediation agent, adsorbent, etc. CaO nanoparticles were obtained by the microwave irradiation technique, using Ca(NO3)2 ⋅ 4H2O and NaOH as starting materials. The formation of monocrystalline CaO nanoparticles was confirmed by the XRD (X-ray diffraction) and TEM (transmission electron microscopy) as well as by SAED (selected area electron diffraction) analysis. The structure of the CaO nanocrystal was found to be cubic with particle size, 24 nm and surface area, 74 m2/g.