Polycrystalline samples of isostructural MSb2O4 (M = Co, Ni) have been prepared by solid state synthesis and lithium-storage is investigated as possible anode materials for lithium-ion batteries. The reaction mechanism of lithium with MSb2O4 (M = Co, Ni) is explored by galvanostatic cycling, cyclic voltammogram and ex situ studies. Both CoSb2O4 and NiSb2O4 exhibit similar electrochemical behavior and show reversible capacity of 490 and 412 mAh g(-1) respectively in the first cycle. Reversible alloying de-alloying of LixSb takes place in an amorphous matrix of M (Co, Ni) and Li2O during electrochemical cycling. (C) 2012 Elsevier Ltd. All rights reserved.