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This was very useful for comparative studies of Different types of XRD and Williamson and Halls methods, the average crystallite size was estimated.The paper deals with the exhaustive study and analysis of VO2+ ions doped ZnS/CdS composite nanopowder with the help of X-ray peak profile analysis (XPPA). The investigation has been carried out by applying a distinct pattern of Williamson-Hall (W-H) approach viz., uniform deformation model, the uniform stress deformation model and uniform deformation energy density model, and size strain plot (SSP). Fourier transforms infrared spectroscopy (FT-IR), scanning electron microscope and energy dispersive spectra (EDS) and transmission electron microscope (TEM) techniques. The XRD study is high manipulated order and fundamental focus is on phase identification, with some analysis on advanced concepts such as crystallite size and lattice strain have been estimated using the modified form of the W-H methods. XRD pattern confirmed that the structure of the sample belongs to the cubic system.