Tin-based intermetallic compounds of different compositions and with micro and nano-sized particles are studied as electrodes for lithium ion batteries. Crystalline microsized particles of CoSn x are obtained at high temperatures, while crystalline nano-sized particles are obtained at low-temperature following a one-pot method which is based on TEG solvent and reduction with NaBH4. The observed capacities of CoSn x compounds in lithium test cells depend on the tin content, electrochemical cycling conditions and crystallite size. The change of the 119Sn Mössbauer isomer shift upon the electrochemical reaction with lithium is more limited for the intermetallic compounds CoSn x than for pure Sn. Nano-sized CoSn x materials show superior specific capacity than microsized CoSn x powders. The maximum observed reversible capacity of nano-Co3Sn2 is equal to 544mAhg−1 in the first cycle, while 413mAhg−1 were observed for nano-CoSn.