NiFe2O4 nanoparticles have been synthesized using the flash auto-combustion technique, while TiO2 nanoparticles were prepared via sol–gel method. NiFe2O4/TiO2 nanocomposite was obtained through the sonochemical method. Investigated samples have been studied through XRD, FTIR, and FESEM. The crystallite sizes of NiFe2O4, TiO2, and NiFe2O4/TiO2 are 48.37, 25.56, and 32.46 nm, respectively. FTIR analysis was used to look into the materials’ functional groups. The images of FESEM illustrated that the particles were prepared in nanoscale. All samples were good absorbers in the UV spectrum through the wavelengths of 200–350 nm. The energy band gap values of TiO2, NiFe2O4, and NiFe2O4/TiO2 nanocomposite are 3.4, 2.3, and 2.5 eV, respectively, for the indirect transition. The samples’ dielectric characteristics have been investigated and they have a semiconductor like behavior. VSM and the Faraday technique were used to test the materials’ magnetic characteristics.