Abstract CoFe2O4 nanoparticles have received immense attention in recent times due to their interesting magnetic properties and they possess good thermal and chemical stability. In the present study, CoFe2O4 nanoparticles have been synthesized via a novel thermal decomposition approach using Co–Fe glycolate precursors. The Co–Fe glycolates were prepared by refluxing the corresponding metal salts in ethylene glycol. The morphology of CoFe2O4 nanoparticles can be tailored by varying the synthesis temperature of Co–Fe glycolates and also the amount of ethylene glycol used. The morphology of CoFe2O4 changes from nanorods to hexagonal particles on changing the synthesis temperature of Co–Fe glycolates from 160 °C to 220 °C, On the other hand, on increasing the amount of ethylene glycol while keeping the synthesis temperature constant (220 °C), the morphology of CoFe2O4 nanoparticles changes from hexagons to octahedra. The Co–Fe glycolates and the CoFe2O4 nanoparticles were characterized using several analytical techniques. The magnetic properties of CoFe2O4 nanoparticles were studied by vibrating sample magnetometry. The CoFe2O4 nanoparticles exhibit high coercivity at 5 K with moderate saturation magnetization.