For preparing calcium ferrite, calcium tris (dmaleato) ferrate(III) precursor was prepared by mixing aqueous solutions of iron(III) maleate, calcium maleate and maleic acid. Various physico-chemical techniques i.e. TG, DTG, DTA, Mössbauer, XRD, IR etc have been used to study the decomposition behaviour from ambient to 900°C and ferrite formation. Three consecutive decomposition steps leading to the formation of α-Fe₂O₃ and calcium carbonate have been observed at various stages of thermolysis. In the final stage the ferrite, bdCa₂Fe₂O₅, is obtained as a result of solid state reaction between α-Fe₂O₃ and calcium carbonate at 788°C, a temperature much lower than for ceramic method. The results have been compared with those of the oxalate precursor.