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Main observation and conclusion: Transition metal‐rare earth oxide catalysts had the ability to catalyze ammonia decomposition according to recent years' scientific reports. However, most of those catalysts had their own limitations: the catalytic activity was poor, and/or the active species could not clearly be identified. Here we report the CoaSmbOx catalysts with good dispersion, controllable content, and excellent catalytic performance for ammonia decomposition. The various content catalysts were synthesized by aerosol‐assisted self‐assembly approach. These catalysts had high dispersion and great morphology according to the images of the transmission electron microscope (TEM) and the scanning electron microscope (SEM). The temperature‐programmed reduction by hydrogen (H2‐TPR) and in‐situ X‐ray diffraction (XRD) results indicated that the interaction between cobalt oxide and samarium oxide influenced the redox properties of cobalt oxide. Combined with in‐situ Raman, we found that Co0 was an active species of the CoaSmbOx catalysts in ammonia decomposition. Moreover, the temperature‐programmed desorption of NH3 (NH3‐TPD) data illustrated that the addition of Sm was beneficial to the adsorption of NH3. In general, we successfully obtained the CoaSmbOx catalyst with high activity and good stability. More importantly, we have identified the structure‐function relationship of catalysts by exploring the active species in the reaction process. [ABSTRACT FROM AUTHOR]