Nickel substituted lithium nano ferrites with the chemical composition Li0.5-0.5x Nix Fe2.5-0.5x O4 (0.0 < x <1.0), were prepared by Citrate-gel method. The single phase cubic spinel structure of the ferrites was confirmed by X-ray diffraction analysis(XRD). In this method,by increasing of Ni composition in the Li-Ni ferrites, Lattice parameter of the prepared samples was increased.Fourier transform infrared spectroscopy (FT-IR) shows the two significant absorption bands in the wave number range of 400-600 cm-1 arising due to the inter-atomic vibrations in the tetrahedral and octahedral coordination compounds. In another method,manganese substituted lithium nano ferrites, Li0.5–0.5xMnxFe2.5–0.5xO4, (0.0 < x <1.0), were prepared by using ceramic method. Single phase cubic structure was confirmed by XRD technique. The lattice parameter “a” was found to increase with increasing Mn2+ ion substitution. The FTIR spectra of these samples were recorded from 200 to 1000 cm−1.The two primary bands corresponded with tetrahedral υA and octahedral υB were observed at about 575 cm−1 and 370 cm−1