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Temperature can govern morphologies, structures and properties of products from synthesis in solution. A reaction in solution at low temperature may result in different materials than at higher temperature due to thermodynamics and kinetics of nuclei formation. Here, we report a low-temperature solution synthesis of atomically dispersed cobalt in a catalyst with superior performance. By using a water/alcohol mixed solvent with low freezing point, liquid-phase reduction of a cobalt precursor with hydrazine hydrate is realized at −60 °C. A higher energy barrier and a sluggish nucleation rate are achieved to suppress nuclei formation; thus atomically dispersed cobalt is successfully obtained in a catalyst for oxygen reduction with electrochemical performance superior to that of a Pt/C catalyst. Furthermore, the atomically dispersed cobalt catalyst is applied in a microbial fuel cell to obtain a high maximum power density …