Herein, we construct amorphous molybdenum oxide films by thermal atomic layer deposition (T‐ALD) and plasma enhanced atomic layer deposition (PE‐ALD). The physical and chemical properties of molybdenum oxide films prepared by the two methods were systematically compared by means of film growth law, atomic force microscope and scanning electron microscope etc. The results show that the amorphous molybdenum oxide physical phase prepared by both atomic layer deposition methods is MoO3. Compared with T‐ALD MoO3, the growth rate of MoO3 thin films prepared by PE‐ALD is higher. Compared to PE‐ALD MoO3, the MoO3 films prepared by T‐ALD did not have nucleation delayed to a laminar growth mode, resulting in smoother deposited films and contained less impurity carbon. The MoO3 prepared by PE‐ALD contains 7.4% impurity carbon. This carbon‐doped film significantly improves the conductivity of the MoO3 film and shows good electrochemical activity. As expected, the MoO3 films prepared by PE‐ALD show good electrocatalytic oxygen evolution reaction. The overpotential was only 259 mV at 10 mA cm‐2 and continued to evolution oxygen for 60 h with almost no attenuation, indicating that carbon doping significantly improves the catalytic intrinsic activity and stability of MoO3.This article is protected by copyright. All rights reserved.