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The article presents the results of optical, electron microscopic and electron microprobe studies of columbite group minerals, collected during heavy mineral concentrate sampling of alluvial deposits in the Mayoko region (Republic of the Congo). The aim of the study is revealing tantalum niobates ore body in this region. We found that these minerals in loose deposits are represented by two grain-size groups: less than 1.6 mm (fine fraction) and 1.6-15 mm (coarse fraction). The grains of both fractions belong mainly to columbite-(Fe), less often to columbite-(Mn), tantalite-(Mn) and tantalite-(Fe), contain impurities of Sc, Ti, and W. The crystals have micro-scaled zoning (zones varies slightly in the Ta/Nb ratio values) and contains a lot of mineral inclusions and veins represented by zircon, pyrochlore supergroup minerals and others. Columbite-(Fe) and columbite-(Mn) are characterized by an increased content of Ta2O5 up to the transition to tantalite-(Fe) and tantalite-(Mn). This allows us to exclude the formation of subalkaline rare-metal granites, their metasomatites (albitites and greisenes) and carbonatites, from the list of possible columbite ore rocks source in the Mayoko district. Thus, beryl type and complex spodumene subtype rare-element pegmatites of the mixed petrogenetic family LCT-NYF (according to P.Černý) should be considered as a probable root source. The results of the research should be taken into account when developing the methodology for prospecting in this area.