ZnO codoped with Mg and Cd in various proportions were prepared by chemical method and annealed at 600 C. The structural and optical properties of these oxide samples were systematically studied by XRD, SEM, EDS and PLspectrometer. XRD pattern shows a hexagonal wurtzite structure. The size of particle as shown by XRD machine and calculated by SchererÂs formula are found in the nano range. The formation of particles showed that they were polycrystaline. Due to large ionic and covalent radii of Cadmium than those of Zinc a lattice deformation occurs with development of strain field. New phases were observed in XRD pattern of few samples. SEMmicrograph show the formation of nanoparticles. EDS study confirm the codoping of ZnO with Mg and Cd. Optical properties like photoluminescence emission showed a blue shift in peak wavelength. General conductivity and photoconductivity was found high in sample containing certain proportion ofMg and Cd in comparison with pure ZnO.