The cubic ZnFe 2 O 4 with the spinel structure is prepared by the urea combustion method. Powder X-ray diffraction and HR-TEM studies confirm the single-phase nature with particle size in the range, 100–300nm. A stable and reversible capacity, 615(±10)mAhg −1 (5.5moles of Li per mole of ZnFe 2 O 4 ) when cycled in the range, 0.005–3.0V vs. Li at a current of 60mAg −1 (0.1C) has been achieved between 15 and 50 cycles. The underlying reaction mechanism contributing to the observed capacity is the combination of ‘de-alloying–alloying’ and ‘conversion’ reactions of ‘LiZn–Fe–Li 2 O composite’. Ex situ HR-TEM and SAED data on the charged-electrode confirmed the proposed reaction mechanism.