Synthesis of Ultrafine Cobalt Ferrite by Thermal Decomposition of Citrate Precursor

Ultrafine particle of CoFe2O4 has been synthesized using citrate precursor technique. Thermal decomposition of the citrate precursor, Co3Fe6O4(C6H6O7)8·6H2O, was investigated by TG, DTA and DTG techniques, gas and chemical analyses and was found to decompose in one or two major steps depending on the heating rate in static/flowing air atmosphere. In the lower heating rate (5°C min-1), metastable acetonedicarboxylate complex was isolated with the evolution of CO gas and coordinated water molecule in the temperature range of 120-220°C. Complete decomposition of the citrate network occurs between 220-330°C with the simultaneous evolution of CO2 and acetone. However both these steps appeared as simultaneous and/or single step process (between 120-160°C), when the heating rate is high (10°C min-1 and above). The ultrafine CoFe2O4 particles are observed as the aggregates having surface area 133.8 m2 g-1 composed of 4.8 nm crystallites. The citrate precursor and the decomposed products were characterized by IR, NMR, XRD, SEM and surface area measurements. This revised version was published online in July 2006 with corrections to the Cover Date.