LiFePO4 was prepared using a melt casting technique of Li2CO3 and FePO4 precursors at 1000 degrees C. The product was characterized by X-ray diffraction and is of the olivine structure with a minor amount of Li4P2O7 impurity. The synthesis, based on a molten procedure, provides a route to large-scale synthetic practices and reduced cost through the use of inexpensive precursors and short reaction times. The large particle sizes of the LiFePO4 crystals obtained from the melt casting were reduced to 200 nm by a series of successive milling techniques without affecting the purity of the sample. A subsequent carbon coating on this milled material with a variety of carbon precursors was capable of producing samples with high capacities and electrochemical results similar to that of commercial LiFePO4 powders. These results indicate that the melt casting procedure could be a competitive synthetic technique for the large-scale production of LiFePO4.