The main objective of this work was to investigate the influence of the order of component synthesis of zinc ferrite–titania nanocomposites on their structural, morphologic, textural, light absorption properties, and performances as photocatalysts. In this respect, nanocomposite materials with 10ZnFe₂O₄-90TiO₂ (wt %) composition were prepared via a two-step synthesis procedure by alternating the order of the component addition during the preparation protocol and characterized by X-ray diffraction, transmission electron microscopy, energy dispersive X-ray, small-angle X-ray scattering, nitrogen sorption, and UV–vis diffuse reflectance spectroscopy. The photocatalytic activity of nanocomposites was evaluated on Rhodamine 6G degradation under visible light illumination. The photocatalytic performances of nanocomposites were clearly superior to the classical TiO₂. Nevertheless, preparing titania in the presence of a presynthesized zinc ferrite led to superior characteristics in terms of band gap value, specific surface area, and grain sizes crucial for the enhancement of the photocatalytic performances.