A series of Bismuth doped Cobalt nanoferrites of chemical composition CoBixFe2-xO4 (where x = 0.00, 0.05, 0.10, 0.15, 0.20 & 0.25) were prepared by sol-gel combustion method and calcinated at 600℃. The structural and morphological studies were carried out by using X-ray diffraction (XRD), Scanning Electron Microscope (SEM), Transmission Electron Microscopy (TEM), Energy Dispersive Spectroscopy (EDS) and Fourier Transform Infrared (FT-IR) spectra showing the single phase spinal structure. The X-ray diffraction (XRD) analysis confirmed a single phase fcc crystal. The crystallite size of all the compositions was calculated using Debye-Scherrer equation and found in the range of 17 to 26 nm. The lattice parameters were found to be decreased as Bi3+ ion doping increases. The surface morphology was studied by Scanning Electron Microscope (SEM) and particle size was confirmed by Transmission Electron Microscopy (TEM). The EDS plots revealed existence of no extra peaks other than constituents of the taken up composition. The Fourier Transform Infrared (FT-IR) studies were made in the frequency range 350 - 900 cm-1 and observed two strong absorption peaks. The frequency band is found at 596 cm-1 where as the lower frequency band at 393 cm-1. It is clearly noticed that the two prominent absorption bands were slightly shifted towards higher frequency side with the increase of Bi3+ ion concentration.
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