The preparation of few layered 3D material Molybdenum/Polyaniline (MoS 2/PANI) nanofiber (NF) composite synthesis via a hydrothermal process. MoS 2/PANI nanofiber composite was characterized via Fourier-transform infrared (FT-IR) spectra to study the chemical functional group and their interaction, and optical properties examine by the UV-visible spectra. Formation of nanosheet and 3D hierarchical flower morphology was examined through Field emission scanning electron microscopy (FESEM), and the elemental analysis examined through Energy-dispersive x-ray (EDX), and Transmission electron microscopy (TEM). XRD studies show the properties of crystalline nature of the nanocomposite. Binding energy and composite elemental identified states measured through x-ray photon spectroscopy (X-PS). The Electrochemical technique was used to investigate cyclic voltammetry, and electrochemical catalytic activity evaluated from EIS which obtained resistance is 137.52 Ω, 66.40 Ω, and 15.25 Ω respectively. Linear sweep voltammetry, CV oxidation peak reached maximum oxidation current is 2.72× 10–4 Amperes, and curve appeared between− 4.5 to 4.5 Volt. Finally MoS 2-PANI-1 Nanofiber composite is prominent material for electrochemical performance.