A binary polyaniline/TiO2 and varied weight ratio TiO2/PANI nanocomposite was successfully fabricated as an electrode for energy storage application. The TiO2 nanoparticles were synthesized via manual irradiation system with wavelength 256 nm and power 125 W. Polyaniline/TiO2 was then prepared by in situ polymerizing TiO2 onto aniline monomer. Polyaniline nanofibers are loaded with TiO2 to product core-shell system. The polyaniline/TiO2 nanocomposite were characterized using XRD, XPS, TEM, TGA, CP and LCR measurements. The structure properties were examined by XRD and XPS, which confirmed preparing polyaniline/TiO2 binary nanocomposite. The thermal stability was investigated using TGA and obtained high stability of polyaniline/TiO2 compared with polyaniline, while the electrochemical properties were examined by LCR measurements. The LCR measurements were appeared dielectric constant and dielectric loss for incorporating TiO2 through PANI. Varied weights ratio TiO2 was worked in increasing the stored energy ability of polyaniline. Notably, the electrochemical investigate results appear that the PANI/TiO2 has a high specific capacitance (250 F/g) compared with pure PANI (200 F/g). KEY WORDS: Supercapacitor, UV irradiation, XPS, LCR, nanofibers Bull. Chem. Soc. Ethiop. 2024, 38(4), 1177-1188. DOI: https://dx.doi.org/10.4314/bcse.v38i4.28