Nano-crystalline CoFe2O4 particles were synthesized through thermal decomposition o of cobalt tartrate- ferric tartrate at 250, 450, 750 and 1050 C. The samples were characterized by XRD, DSC-TG, SEM, TEM and FT-IR. The XRD analysis showed that the sample calcined o at 1050 C exhibit pure spinel phase. The crystallite sizes lie in the range of 30 – 61 nm. The samples obtained at different calcination temperatures have different morphologies. The kinetics of thermal decomposition of metal tartrate mixtures were studied using non-isothermal thermogravimetric techniques. The thermal decomposition proceeds in three steps for cobalt iron (III) tartrate. The kinetic analysis of non-isothermal data of the decomposition reaction is best described by the Random nucleation in (three-dimentions) (A4) models. The activation parameters were calculated and the results of the dynamic integral methods were compared and discussed.