Electrochemical ammonia synthesis from N2 under mild condition is considered a promising strategy to store energy produced by renewable sources, but it is affected by the lack of efficient catalysts for nitrogen reduction. In this work Fe-based nanoparticles with different morphology are deposited on carbon cloth via drop-casting and chemical reduction. The catalyst activity has been evaluated by cyclic voltammetry and chronoamperometry, using a 0.01 M phosphate buffered electrolyte (PBS). The produced ammonia has been determined through the indophenol method. As effective strategy to improve the catalytic activity, the morphology and particle size have been optimized and an electrochemical activation procedure has been implemented. Activation increases the available active sites and is related to higher amount of oxygen vacancies and Fe+2/Fe+3 ratio. Catalysts with optimized morphology produce …