Transition metal oxides formed by a single or heterogeneous combination of transition metal ions and oxygen ions have various types of crystal structures, which can be classified as layered structures and non-layered structures. With non-layered structures, it is difficult to realize a two-dimensional structure using conventional synthesis methods. In this study, we report the synthesis of cobalt oxide into wafer-scale nanosheets using a surfactant-assisted method. A monolayer of ionized surfactant at the water-air interface acts as a flexible template for direct cobalt oxide crystallization below. The nanosheets synthesized on the water surface can be easily transferred to an arbitrary substrate. In addition, the synthesizing morphological and crystal structures of the nanosheets were analyzed according to the reaction temperatures. The electrochemical properties of the synthesized nanosheets were also measured at each temperature. The nanosheets synthesized at 70 °C exhibited higher catalytic properties for the oxygen evolution reaction than those synthesized at other temperatures. This work suggests the possibility of changing material performance by adjusting synthesis temperature when synthesizing 2D nanomaterials using a wide range of functional oxides, resulting in improved physical properties.