The present invention relates to a method for preparing an electroactive metal polyanion or a mixed metal polyanion comprising forming a slurry comprising a polymeric material, a solvent, a polyanion source or alkali metal polyanion source and at least one metal ion source; heating said slurry at a temperature and for a time sufficient to remove the solvent and form an essentially dried mixture; and heating said mixture at a temperature and for a time sufficient to produce an electroactive metal polyanion or electroactive mixed metal polyanion. The electrochemically active materials so produced are useful in making electrodes and batteries.