This study presents the successful electrodeposition of polyaniline (PANI) and TiO₂/PANI composites on boron-doped diamond (BDD) and fluorine-doped tin oxide (FTO) substrates via cyclic voltammetry. Using 20 scan cycles in 0.5 M H₂SO₄, we synthesized thin films with tailored electrochemical properties. The formation of PANI was confirmed by characteristic redox peaks in the voltammograms, while FTIR spectroscopy identified key functional groups and bonding interactions between TiO₂ and PANI. Morphological analysis via optical and scanning electron microscopy revealed uniform but cracked surfaces influenced by TiO₂ loading. Composite electrodes with molar ratios of 2:1, 4:1, and 6:1 (TiO₂:PANI) were compared, showing increased titanium content with higher ratios, as confirmed by EDS. This work offers a reproducible route for designing modified electrodes with enhanced interfacial properties.