Nanostructured Li2FeSiO4/C was synthesized by high-energy ball-milling and the amorphous citrate-assisted techniques. Similar redox behaviour is observed for samples prepared by the amorphous citrate-assisted route followed by a 4 h heat treatment: 0.3 V polarization and more sloping behaviour was observed when cycling between 2.0 V and 3.7 V at 60 °C; lower capacity fade is also observed compared to Li2FeSiO4/C prepared by the solid-state reaction technique. A discharge capacity of 102 mA h g− 1 is obtained for samples prepared by the high-energy ball-milling method, while capacities decrease from 95 to 77 mA h g− 1 using the amorphous citrate method for heat-treatment times increasing successively from 4 h to 18 h.