Co-Mn-O composite oxide nanosheet catalyst was successfully prepared using a facile urea-assisted one-step hydrothermal method in the absence of organic or organic templating reagent. Co-Mn-O nanosheet catalyst was optimized by varying hydrothermal process parameters such as molar ratio of Co-Mn to urea, hydrothermal temperature, and hydrothermal time. Various characterization techniques including scanning electron microscopy, X-ray diffraction, nitrogen adsorption, X-ray photoelectron spectroscopy, Raman spectroscopy, and H 2 temperature-programmed reduction were used to reveal the relationship between catalyst nature and catalytic performance in CO preferential oxidation (CO PROX) in excess H 2 . The developed Co-Mn-O nanosheet catalyst have demonstrated much superior catalytic performance to Co-Mn-O nanoparticle, particularly in the low temperature range, and 100% CO conversion over the developed Co-Mn-O nanosheet can be achieved in temperature range of 50 to 150 C at 10,000 mL g 21 h 21 of gas hourly space velocity in the standard feed. Furthermore, the almost complete CO removal over Co-Mn-O nanosheet at 125 C of low temperature with 94.9% selectivity can be achieved even in the simulated reformed gas. The excellent catalytic performance is ascribed to nanosheet morphology, more surface Co 31 , smaller average crystallite size, higher reducibility, and strong Co-Mn interaction. Catalytic stability investigation indicates the developed nanostructured catalyst exhibits high catalytic stability for CO PROX reaction in simulated gas. The developed Co-Mn-O nanosheet catalyst can be a potential candidate for catalytic elimination of trace CO from H 2 -rich gas for Proton exchange membrane fuel cell applications. Reaction conditions: 100 mg catalyst, GHSV 5 15,000 mL h 21 g 21 , 1.0 vol % CO, 1.0 vol % O 2 , 50 vol % H 2 , Ar balance. [Color figure can be viewed in the online issue, which is available at wileyonlinelibrary.com.] 242 Figure 8. The CO conversion (a) and O 2 selectivity to CO 2 (b) over the Co-Mn-O-ns samples prepared with diverse n Co-Mn/Urea . Reaction conditions: GHSV 5 15,000 mL h 21 g 21 , 1.0 vol % CO, 1.0 vol % O 2 , 50 vol % H 2 , Ar balance. [Color figure can be viewed in the online issue, which is available at wileyonlinelibrary.com.]