Abstract: Multifunctional core@shell nanoparticles have been synthesized in this paper through 3 stages: NiFe2O4 nanoparticles by microwave irradiation using Pedalium murex leaf extract as a fuel, core@shell NiFe2O4@TiO2 nanoparticles by sol-gel, and NiFe2O4@TiO2@rGO by sol-gel using preprepared reduced graphene oxide obtained by modified Hummer’s method. XRD analysis confirmed the presence of both cubic NiFe2O4 spinel and tetragonal TiO2 rutile phases, while Raman spectroscopy analysis displays both D and G bands (ID/IG = 1.04) associated with rGO. Morphological observations by HRTEM reveal a core-shell nanostructure formed by NiFe2O4 core as confirmed by SAED with subsequent thin layers of TiO2 and rGO. Magnetic measurements show a ferromagnetic behavior, where the saturation magnetization drops drastically from 45 emu/g for NiFe2O4 to 15 emu/g after TiO2 and rGO nonmagnetic bilayers coating. The as-fabricated multifunctional core@shell nanostructures demonstrate tunable self-heating characteristics: rise of temperature and specific absorption rate in the range of ΔT = 3–10°C and SAR = 3–58 W/g, respectively. This effectiveness is much close to the threshold temperature of hyperthermia (45°C), and the zones of inhibition show the better effective antibacterial activity of NTG against various Gram-positive and Gram-negative bacterial strains besides simultaneous good efficient, stable, and removable sonophotocatalyst toward the TC degradation.