The decomposition of the Ethiopian Kenticha tantalite ore was studied using the KOH fusion and H2O leaching system at 400 0C for a 1 h reaction time. The experimental results obtained showed that 27 wt% of Ta2O5 was mainly transformed into insoluble KTaO3, not to be KNbO3, and as well, into the dissolved liquor containing 94.73 vol% of Nb2O5 and 75.80 vol% of Ta2O5. The observations, supported by the EDXRF, XRD, and ICP-OES techniques, showed that the ratio of the dissolved mixture of Nb and Ta metal ions was beneficial to the solvent extraction from both Ta2O5 and Nb2O5. Niobium and tantalum were extracted from their neutralized alkaline dissolved and hydrolyzed solution by a new process using the EMIC/AlCl3 ionic liquid as the extractant using selective stripping, precipitation, and calcination of a highly crystalline pure 99.84 wt% of Nb2O5 and amophours 90.81 wt% of Ta2O5. The compositions of the dissolved metal ions and solids were analyzed by the ICP-OES, EDXRF, XRD, and FT-IR techniques.