Abstract: Organoclay is an organic-inorganic composite that is consists of layers of two tetrahedral silica sheets and one octahedral alumina sheet pillared by organic reagents to improve the physical and chemical properties. We report the synthesis of CeO2/organo-clay nanocomposite with a uniform distribution of particles in morphology by a programmed method of microwave heating reaction. Cerium nitrate hexahydrate as an initial metal source was added to the dispersed organoclay in aqueous solution and then transferred into a domestic microwave oven with a power of 900 W for 20 min. the synthesized nanocomposite was characterized by using Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersion of x-ray spectrometry (EDX) techniques. XRD pattern clearly revealed the formation of the CeO2/ organoclay nanocomposite having pillared planes. Scanning electron microscopy (SEM) images of the resulting product indicated a uniform morphology of nano-sized particles with an average size of 33 nm. The composition of the resulting product into a matrix of resin epoxy in different weight ratios was studied.