A series of iron−niobium composite oxides for selective catalytic reduction of NO x with NH 3 (NH 3 -SCR) were prepared by coprecipitation with the assistance of CTAB. The obtained FeNb 0.4 O x -C catalyst exhibited superior SCR performance, with NO x conversion above 90% at 250−400 °C under a high GHSV of 250 000 h −1 . Characterization of the oxides by N 2physisorption, XRD, Raman, TG/DTA, NH 3 -TPD, H 2 -TPR, and XPS showed that when CTAB was present during preparation, a strong interaction between Fe and Nb was produced for the Fe− Nb catalysts made with an appropriate proportion of the two elements, which promoted the formation of γ-Fe 2 O 3 . The strong Fe−Nb interaction not only induced more reducible Fe at low temperatures but also enhanced the surface acidity, both of which brought about more active sites on the FeNb 0.4 O x -C catalyst. Owing to such strong interaction between redox-acid sites, more NO x species were adsorbed and activated over FeNb 0.4 O x -C, thus exhibiting high reactivity during the NH 3 -SCR reaction, which was revealed by DRIFT and kinetic studies.