Conductive polymer nanocomposites are attracting increasing interest for their potential in advanced optoelectronics, sensing, and energy applications, owing to their tunable electrical and optical properties. In this study, we present the fabrication and characterisation of novel PANI-CSA nanocomposite films doped with cobalt (Co), nickel (Ni), and a combination of Co–Ni nanoparticles. These materials were synthesised via chemical polymerisation in a camphor sulfonic acid (CSA) solution. Structural, optical, and electrical properties were systematically examined using four-point probe measurements, X-ray diffraction, scanning electron microscopy, and ultraviolet–visible (UV–Vis) spectroscopy. Our findings demonstrate that doping with Co and Ni nanoparticles reduces the optical bandgap, enhances electrical conductivity, and improves UV–visible light absorption. Theoretical modelling of surface plasmon resonance using the Kretschmann configuration further revealed that co-doping with Co and Ni significantly enhances sensitivity, positioning these films as promising candidates for plasmonic biosensing. The integration of dual-metal doping with CSA protonation in PANI offers an innovative approach for developing multifunctional nanocomposites tailored for advanced photonic and sensing applications.
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