Hybrid films for applications in organic electronics from NiFe2O4nanoparticles (NPs) in poly(3,4 ethylene dioxythiophene), poly(4-styrenesulfonate) (PEDOT:PSS), and poly(methyl methacrylate) (PMMA) were fabricated by the spin-coating technique. The films were characterized by infrared spectroscopy, atomic force microscopy, scanning electron microscopy, and energy-dispersive spectroscopy to subsequently determine their optical parameters. The electronic transport of the hybrid films was determined in bulk heterojunction devices. The presence of NiFe2O4NPs reinforces mechanical properties and increases transmittance in the hybrid films; the PEDOT:PSS-NiFe2O4NPs film is the one that has a maximum stress of 28 MPa and a Knoop hardness of 0.103, while the PMMA-NiFe2O4NPs film has the highest transmittance of (87%). The Tauc band gap is in the range of 3.78–3.9 eV, and the Urbach energy is in the range of 0.24–0.33 eV. Regarding electrical behavior, the main effect is exerted by the matrix, although the current carried is of the same order of magnitude for the two devices: glass/ITO/polymer-NiFe2O4NPs/Ag. NiFe2O4NPs enhance the mechanical, optical, and electrical behavior of the hybrid films and can be used as semi-transparent anodes and as active layers.