Nano sized Sn based alloy materials were prepared by mechanical milling using Ti, Al and Mg as the reducing agent and different grinding media. It was found, that both the reductive metal and grinding media significantly affect the material formed and the resulting electrochemical behavior. Titanium reduction provided materials with excellent capacity, 600 mAh/g close to the theoretical capacity, and capacity retention on cycling. The electrochemical behavior was further enhanced by the use of iron grinding media, which resulted in the alloying of some or all of the tin with iron giving Sn(2)Fe. The capacity and rate capability of these iron containing materials is comparable to those of the SnCo-C compounds. (C) 2011 The Electrochemical Society. [DOI: 10.1149/2.108112jes]