Polypyrrole (Ppy) and Ppy/Ni(OH) 2 -NiO nanocomposite are prepared through the in situ polymerization oxidation reaction (on glass), in which the composite is formed through the oxidation of NiSO 4 . The prepared materials were characterized to reveal their morphology, chemical structure, and optical properties.The Ppy and Ppy/Ni(OH) 2 -NiO have average particle sizes of 160 and 250 nm, respectively. Moreover, the bandgap values are 1.70 and 1.44 eV, respectively.Through the composite, the polymer acts as a shell (40 nm), while the Ni(OH) 2 -NiO is the core. Analysis of the Ppy illustrates that the crystalline nature of the polymer increases after the composite formation, in which the pure Ppy has no sharp peaks, while the characteristic two peaks are formed after the composite formation. Moreover, a hexagonal Ni(OH) 2 is confirmed inside the composite.The applications of the glass/Ppy and glass/Ppy/Ni(OH) 2 -NiO are carried out as optoelectronic devices, in which the testing is carried out under light/dark and monochromatic wavelengths light, the J ph values are 0.12 and 0.85 mAÁcm À2 , respectively. The photoresponsivity (R) for the composite optoelectronic is 12.5 mAÁW À1 while the detectivity (D) is 2.79*1011 Jones.