A nanostructured composite with overall atomic composition Ni0.14Sn0.17Si0.32Al0.037C0.346 has been prepared combining powder metallurgy and mechanical milling techniques for being used as anode material in Li-ion battery. Chemical and structural properties of the nanocomposite have been determined by Xray diffraction (XRD), Sn-119 Transmission Mossbauer Spectroscopy (TMS), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The composite consists of Si particles with typical size similar to 150 nm embedded in a poorly crystallized and complex multielemental matrix. The matrix is composed mostly by Ni3.4Sn4, and disordered carbon. Electrochemical evaluation shows a high reversible capacity of 920 mAh g(-1), with reasonable reversible capacity retention (similar to 0.1% loss/cycle) over 280 cycles. (C) 2011 Elsevier B.V. All rights reserved.