LiFeSO4F, which can be synthesized either via an ionothermal or solid-state route, stands as a possible alternative to LiFePO4 for the next generation of Li-ion batteries. Here we demonstrate a different route to prepare this material. It consists of (i) combining stoichiometric amounts of FeSO4F center dot nH(2)O and LiF in a powdered polymeric media, which has a low melting point and remains stable up to 300 degrees C, and (ii) recovering and purifying the reacted powder by washing it in organic solvent. This method offers advantages in terms of both cost and kinetics while providing powders that have similar performances vs Li. (C) 2010 The Electrochemical Society. [DOI: 10.1149/1.3477936] All rights reserved.