Ternary compositions of LiFeO 2 , LiCoO 2 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 LiFeO 2 –LiCoO 2 –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 LiFeO 2 –NiO binary system and five ternary sub-systems, each with a constant molar ratio of LiFeO 2 /NiO while varying LiCoO 2 content, were studied. Powders with characteristics appropriate for MCFC cathode fabrication could be obtained by the Pechini method. The particle size of LiFeO 2 –LiCoO 2 –NiO powders considerably depends on the calcination temperature and the material composition. The electrical conductivity study reveals the ability of preparing LiFeO 2 –LiCoO 2 –NiO materials with adequate electrical conductivity for MCFC cathode application.