Synthesis and characterization of solid electrolyte structure material using different kinds of lithium and aluminum compounds for molten carbonate fuel cells have been carried out. Synthesis operations are performed using three different kinds of lithium compounds (LiOH center dot H2O, LiNO3 and Li2CO3) and two different kinds of aluminium compounds (Al2O3, Al(OH)(3)). During the synthesis, all the reactions are conducted at four different pH levels (1.5, 4, 9.5 and 12) and are calcinated at three different temperatures in open air conditions. In the light of thermal, structural and surface area characterization (TG-DTA, XRD and BET analyses), it is concluded that LiAlO2 which is produced with Li2CO3 and Al(OH)(3), is found to be convenient.