The present paper report the formation of ZnO/CdO composites via the Sol-Gel technique. The synthesized sample is dried in air and annealed at 300 °C. The heat-treated sample is powdered and structure characterization of obtained powder composite is investigated through X-ray diffraction (XRD) and Rietveld refinement techniques. The crystal structure, morphology, and composition of the powder composite were analyzed in detail. XRD diffractograms were obtained through X-ray diffraction and the Rietveld refinement method is used to estimate the crystalline phases present in the sample using XRD results. The refinement of the prepared samples was done by Fullprof Suite Software. The analysis of diffractograms gives the crystalline nature and refinement gives the presence of ZnO and CdO phases. XRD data was used to find the size and the crystallite size estimated for ZnO is 38.35 nm, and for CdO is 44.09 nm. Refinement suggests that ZnO is hexagonal with space group P36mc (186), while CdO is cubic with space group Fm-3 m (225). Lattice parameters calculated for ZnO are found to be a = b = 3.250, c = 5.213, α = β = 90°, and γ = 120°, and for CdO lattice parameters are found as a = b = c = 4.694, α = β = γ = 90°. The dislocation density of ZnO and CdO is calculated as 0.001012 m/m3 and 0.00081 m/m3. Lattice strain of composite is calculated by W-H plot and found to be (2.06 ± 0.876614) * 103.The inter-atomic distance and Wyckoff positions are also estimated.