NiO nanoparticles that are highly active for the ethane activation have been prepared. These nanoparticles have been dispersed on the surface of two different Nb2O5 materials by using a novel dry nanodispersion method. This article describes the characterization and catalytic behavior of both series of catalysts as well as the nature of the active sites required for the transformation of ethane into acetonitrile and/or ethylene. It is demonstrated how such active sites present in the catalysts are obtained through this novel dry mixing method. The catalysts obtained are promising catalytic materials for both, ethane ammoxidation and oxidative dehydration (ODH) reactions.