Spinel ferrite nanoparticles presents fascinating application on biomedical, which aimed us to focus the recent investigations on synthesis of pure and manganese substituted nickel ferrite (Ni1-xMnxFe2O4; x = 0.0, 0.5) nanoparticles using sol-gel combustion technique. The structure and the average crystallite size of the synthesized nanoparticles were analyzed from Powder X-Ray Diffraction studies. The vibrational bands corresponding to metal-oxygen linkage detected between 300-700 cm-1 were noticed from FT-IR spectral analysis. TEM analysis was used to study the morphology of the synthesized nanoparticles.