This book presents a comprehensive study on the synthesis structural analysis and electrochemical performance of conducting polymers (Polyaniline Polypyrrole) and transition metal oxides (MnO₂ Cr₂O₃) for supercapacitor applications. Emphasis is placed on galvanostatic electrodeposition techniques for fabricating single-layer and bilayer heterostructure thin films on stainless steel substrates.The book systematically explains the growth mechanisms physicochemical characterization (XRD SEM FTIR UV-Vis AFM) and electrochemical evaluation (CV GCD EIS) of individual and composite layers. Special focus is given to bilayer electrodes such as PANI/Cr₂O₃ PPy/MnO₂ and other combinations that demonstrate enhanced capacitance cyclic stability and charge transport behavior.With clear illustrations experimental methods and analysis suitable for both beginners and researchers this book serves as a valuable reference for:Energy storage researchersSupercapacitor and battery technologistsNanoscience and materials science studentsScientists working on polymer-oxide hybrid materialsThe work also highlights structure-property relationships and provides insights into designing next-generation high-performance supercapacitor electrodes.