LiV308 powder has been prepared on a large scale by spray drying ofan aqueous gel. The material was further dehydrated at 150 and 350ºC. These materials were characterized by TGA, XRD and electrochemical methods. Materials dried at 150 and 350ºC, showed an unusual high reversible capacity, close to 4 Li per formula unit, and cycle well. The material dried at 350ºC is very similar to the crystalline LiV308 prepared by conventional high temperature synthesis.