Ternary compositions of LiFeO2LiCoO2 and NiO are expected to posses desirable characteristics for the Molten Carbonate Fuel Cell (MCFC) cathode application. This paper presents a detailed description of the synthesis of LiFeO2-LiCoO2-NiO powders as well as dense sintered materials together with a brief discussion on the common aspects and trends observed in the characterization of these materials for MCFC cathode application. Feasibility of two wet-chemical powder preparation techniques, the Pechini method and the glycine-nitrate method, was investigated to obtain powders with characteristics appropriate for cathode fabrication. Materials in the LiFeO2-NiO binary system and five ternary subsystems, each with a constant molar ratio of LiFeO2/NiO while varying LiCoO2 content, were studied. Powders with characteristics appropriate for MCFC cathode fabrication could be obtained by the Pechini method. The particle size of LiFeO2-LiCoO2-NiO powders considerably depends on the calcination temperature and the material composition. The electrical conductivity study reveals the ability of preparing LiFeO2-LiCoO2-NiO materials with adequate electrical conductivity for MCFC cathode application. (c) 2005 Elsevier B.V. All rights reserved.