Conventional two-dimensional materials either have natural layered structures or are produced, with large surface areas, via physical or chemical synthesis. However, to form a twodimensional material from a non-layered material, a method different from the existing ones is required. In this study, a surfactant-assisted method was utilized to synthesize Zn(OH)2 (a nonlayered transition metal oxide) nanosheets. This study described the synthesis of Zn(OH)2 nanosheets using an anionic sulfate layer and demonstrated a method of controlling the thickness and shape of the synthesized nanosheets by varying the surfactant concentration. Further, the characteristics of oxygen evolution reaction using ZnO/Zn(OH)2 nanosheets, obtained by annealing the synthesized sheets, as catalysts were studied.