Two-dimensional (2D) nanosheets with high surface-to-volume ratios have garnered significant attention for their electrocatalytic properties. This study explores the characterization and electrocatalytic performance of highly porous monometallic platinum (Pt) nanosheets and bimetallic platinum-nickel (Pt3Ni) nanosheets for the hydrogen evolution reaction (HER) in both alkaline and acidic media. Advanced characterization techniques were employed to elucidate the morphological and compositional properties of the Pt and Pt3Ni nanosheets. Electrochemical characterization demonstrated that Pt3Ni nanosheets/C outperformed Pt nanosheets/C and commercial Pt/C in terms of HER activity and stability. The enhanced HER performance of Pt3Ni nanosheets/C is believed to be due to the dominance of the Volmer-Tafel mechanism. These findings highlight the potential of 2D bimetallic nanosheets and suggest a promising avenue for advancing hydrogen energy technologies.