Fe‐doped CoCr oxide catalysts are prepared by solid‐phase mixing method, coprecipitation method, mechanical mixing method, and citric acid method, respectively, and their catalytic activity in the selective catalytic reduction of nitrogen oxides with NH3 (NH3‐SCR) is tested. The Fe0.5CoCrOx catalysts prepared by all preparation methods have good water resistance and sulfur resistance when the calcination temperature is 400 °C. Fe0.5CoCrOx prepared by coprecipitation method by calcination at 400 °C (CP‐400) is shown to have the optimum catalyst activity. In addition, the catalysts are characterized by a series of characterizations. The characterization results show that CP‐400 has the largest specific surface area, which makes the active and acidic sites highly dispersed on the surface of CP‐400, resulting in stronger redox and acidity and improved SCR activity. The removal of NO by NH3‐SCR over CP‐400 at 150 °C follows the Eley‐Rideal (ER) and Langmuir‐Hinshelwood (LH) mechanisms.