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 titania–zinc 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 plasma-assisted 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.