Spinel CdFe2O4 nanoparticles were synthesized using metallic nitrates and PEG using sol-gel method followed by calcination for 2 h at 600 °C. PEG performed as a surfactant. FT-IR spectral analysis, powder XRD, HR-SEM, thermogravimetry /differential scanning calorimetry (TG/DSC) analysis and vibrating sample magnetometer (VSM) were used to study the morphology, structural, thermal and magnetic properties of spinel CdFe2O4 powder. FT-IR spectral results shows that type of bonds between metals and oxygen, XRD results indicated that the resultant particles had crystalline, pure single phase monoclinic CdFe2O4 structure and HRSEM shows that the particles are well defined spherical shaped nano particle.