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 X-ray diffraction (XRD), 119Sn Transmission Mössbauer Spectroscopy (TMS), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The composite consists of Si particles with typical size ∼150nm 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 920mAhg−1, with reasonable reversible capacity retention (∼0.1% loss/cycle) over 280 cycles.