In the past years, an important problem that requires solutions at the global scale is the environmental pollution. This work describes a possible approach toward finding such solutions based on nanophotocatalysts with improved activity. Thus, the present study reports a new and efficient synthesis procedure for titaniaezinc ferrite nanocomposite with enhanced photodegradation activity. The method is based on the liquid phase plasma technique and follows a bottom-up scheme. The resulted materials have been compared with those synthesized by the ultrasound-assisted method. Using the plasmaassisted procedures in the fabrication of an efficient nano(photo)catalyst decreases considerably the reaction time. The liquid phase plasma generates nanoparticles with enhanced structural, textural, and morphological properties as demonstrated by X-ray diffraction, nitrogen sorption, transmission electron microscopy, and small-angle X-ray scattering.