Developing highly efficient Au/TiO₂/WO₃ heterostructures with applications in heterogeneous photocatalysis (photocatalytic degradation) and surface-enhanced Raman spectroscopy (dye detection) is currently of paramount significance. Au/TiO₂/WO₃ heterostructures were obtained via heat or time-assisted synthesis routes developed by slightly modifying the Turkevich–Frens synthesis methods and were investigated by TEM, SEM, XRD, Raman spectroscopy, XPS, photoluminescence, and UV–vis DRS techniques. Structural features, such as WO₃ crystalline phases, TiO₂ surface defects, as well as the WO₃ (220) to TiO₂-A (101) ratio, were the key parameters needed to obtain heterostructures with enhanced photocatalytic activity for removing oxalic acid, phenol, methyl orange, and aspirin. Photodegradation efficiencies of 95.9 and 96.9% for oxalic acid; above 96% (except one composite) for phenol; 90.1 and 97.9% for methyl orange; and 81.6 and 82.1% for aspirin were obtained. By employing the SERS technique, the detection limit of crystal violet dye, depending on the heterostructure, was found to be between 10⁻⁷–10⁻⁸ M. The most promising composite was Au/TiO₂/WO₃-HW-TA it yielded conversion rates of 82.1, 95.9 and 96.8% for aspirin, oxalic acid, and phenol, respectively, and its detection limit for crystal violet was 10⁻⁸ M. Au/TiO₂/WO₃-NWH-HA achieved 90.1, 96.6 and 99.0% degradation efficiency for methyl orange, oxalic acid, and phenol, respectively, whereas its limit of detection was 10⁻⁷ M. The Au/TiO₂/WO₃ heterojunctions exhibited excellent stability as SERS substrates, yielding strong-intensity Raman signals of the pollutant molecules even after a long period of time.

Magnetically separable TiO₂-based composite photocatalysts have gained significant interest in the past two decades; however, the optimization of their synthesis and the stabilization of the magnetic iron oxide within the composite is still an open challenge. The present study investigates the photocatalytic behavior and recyclability of TiO₂-Fe₃O₄ composites, with emphasis on a possible correlation between pollutant degradation efficiency, recyclability, iron oxide stability, and the phase composition of the chosen TiO₂ base. Magnetite nanoparticles were synthesized under varied temperature and alkaline conditions to identify optimal parameters for achieving the desirable magnetic properties. The magnetic nanoparticles were integrated into composite systems with either commercial TiO₂ (Evonik Aeroxide P25 with anatase–rutile mixed phase) or a hydrothermally synthesized anatase TiO₂. The P25-based composite removed 99% paracetamol from aqueous solutions under UV-A irradiation and demonstrated successful recyclability, maintaining 96% paracetamol degradation efficiency after four uses. In contrast, the anatase TiO₂-based magnetic composite exhibited a lower performance (70%) and a significantly hindered recyclability (45% after four cycles). The difference in performance was attributed to variations in the phase composition of the employed TiO₂ in the composites and, consequently, in their charge separation mechanisms.