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The formation of impurity Li(x)Ni(1-x)O when synthesizing spinel LiNi(0.5)Mn(1.5)O(4) using solid state reaction method, and its influence on the electrochemical properties of product LiNi(0.5)Mn(1.5)O(4) were studied. The secondary phase LixNi(1-x)O emerges at high temperature due to oxygen deficiency for LiNi(0.5)Mn(1.5)O(4) and partial reduction of Mn(4+) to Mn(3+) in LiNi(0.5)Mn(1.5)O(4). Annealing process can diminish oxygen deficiency and inhibit impurity Li(x)Ni(1-x)O. The impurity reduces the specific capacity of product, but it does not have obvious negative effect on cycle performance of product. The capacity of LiNi(0.5)Mn(1.5)O(4) that contains Li(x)Ni(1-x)O can deliver about 120 mAhg(-1). (C) 2011 Elsevier B.V. All rights reserved.