A facile chemical route to prepare a well‐defined Ni powder on a mass‐production scale without external heating was suggested. A highly concentrated Ni complex was formed between NiCl2 and N2H4 solution, and subsequent addition of NaOH solution triggered serial reactions from the Ni complex decomposition via Ni(OH)2 formation to the reduction of a Ni(OH)2 gel into well‐defined Ni spheres. The high temperature necessary for the reaction was attained not by external heating but by exothermic reactions such as complex formation and reduction. The preparation of monodisperse and spherical Ni powder was attributed to uniform distribution of the reducing agent (N2H4) within the Ni(OH)2 gel.

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