Composite electrode materials containing nanoparticles of nearly amorphous CoSn and ultrathin layers of graphite are prepared here. For this purpose, Sn(II) and Co(II) ions in tetraethyleneglycol are reduced with NaBH4 in the presence of ball-milled graphite while high-intensity ultrasonication is continuously applied. The followed preparative route is a combination of the polyol and sonochemical methods. The observed capacity value for CoSn-ball milled graphite is over 400 mAh/g after 40 cycles (this is superior to graphite). The good electrochemical cycling behavior is connected to the small particle size of CoSn, the low crystallinity of CoSn and the dispersion of the CoSn particles in an optimized carbon matrix. The selected binder (polyvinylidene fluoride or lithium polyacrylate) also can contribute to improve the cycling behavior. The low electrochemical efficiency, particularly in the first cycles, may be related to the spontaneous oxidation of the metallic particles surface and irreversible electrolyte consumption. The use of inert atmosphere (Ar-flow) results in a decrease of the tin oxide content, as determined by using Sn-119 Mossbauer spectroscopy, an increase of the initial electrochemical efficiency up to a maximum of 90.4%, and higher capacities (507 mAh/g after 40 cycles). (C) 2011 Elsevier Ltd. All rights reserved.