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We herein report a facile two‐pot method to prepare a series of the two‐dimensional Ni(OH)2 nanocrystals with varied surface structures via the in‐situ surface transformation derived from Nickel metal‐organic framework (Ni‐MOF) in KOH solution at room temperature. The Ni(OH)2 obtained at the KOH concentration of 0.25 M displayed superior performance among the samples in terms of activities and stability. Further investigation proves that the enhanced urea oxidation reaction (UOR) activities can be ascribed to the cooperation of the larger electrochemical surface area, a faster electronic transfer speed, and a lower transfer resistance on the surface. These findings provide a new route for the rational design and synthesis of advanced electrocatalysts with relatively lower energy consumption that aims to be large‐scale synthesized and utilized in clean energy conversion and applications. [ABSTRACT FROM AUTHOR]