Lithium trivanadate, LiV3O8, can be prepared in a finely dispersed form by dehydration of aqueous lithium vanadate gels. Two methods of dehydration, both easily adaptable to large-scale production, are described in this work : freeze drying and spray drying. After heat-treatment of the dried gels (xerogels) to remove loosely bound water they show a high capacity for lithium insertion, approaching four additional lithium per formula unit, and good reversibility as electrode materials for high energy density lithium cells. How the heat-treatment temperature influences the crystal structure is demonstrated as well as the electrochemical properties of the vanadium oxide.