Magnesium Oxide (MgO) is an attractive material for a wide range of application such as catalysis, treatment waste and an additive to paints, refractory materials and superconductive materials. It yield significant advantage when it is manufactured and used on a nanoscale dimensions. In this study cubic MgO nanoparticles were prepared by using non-aqueous sol-gel process with good morphology and with limited surface area properties and monodispersity. The nanoparticle was characterized by various analytical techniques such as TEM, SEM, XRD, TGA/DTA, FT-IR and Raman spectroscopy. The average particle size with 43 nm and surface area of 2.81 m 2/g was obtained. The non-aqueous process offers the better understanding for controlling the reaction mechanism at a molecular level with high cyrstallinity and well defined uniform morphologies. © 2012 American Scientific Publishers. All Rights Reserved.