This research focuses on the rational design and electrochemical evaluation of Iron-Nitrogen-Carbon (Fe-N-C) catalysts for the Oxygen Reduction Reaction (ORR) as PGM-free alternatives for Proton Exchange Membrane Fuel Cells (PEMFCs). As PEMFCs gain attention for their efficiency and low emissions, replacing platinum-group-metal catalysts has become essential. Fe-N-C materials offer tunable active-site environments, yet their performance depends strongly on the carbon structure, accessibility of Fe-Nx sites, and synthesis-induced chemical environment. Understanding these factors is critical for enabling their future integration into membrane electrode assemblies (MEAs). The goal of this thesis is to investigate the synthesis, physicochemical properties, and electrochemical behavior of porous Fe–N–C electrocatalysts prepared using an SBA-15 mesoporous silica hard-templating method.