Coupling TiO2 with various elements could enhance its photocatalytic activity. In this study, an innovative ultrasound-assisted sol–gel method was used to synthesize TiO2/Ag(x%) by varying Ag–support mass (x = 9.3, 17.1, and 23.6%), followed by calcination at 450 °C for 30 min. The aim was to demonstrate that Ag compositing improves photoactivity under visible light (>400 nm). The synthesized photocatalysts were assessed for their effectiveness in the degradation and mineralization of Methylene Blue (MB) and Acid Orange 7 (AO7) using visible lamps emitting in the range of 400–800 nm. Characterization of the prepared photocatalysts was performed by using Raman spectroscopy, SEM/EDS, pHpzc, and UV–visible spectroscopy. Raman spectroscopy confirmed the predominance of the anatase phase in all the photocatalysts. The photodegradation efficiencies of the selected dyes, MB and AO7, reached 99% (pH 6) and 95% (pH 3) after 180 min of irradiation, respectively. The best performance for the degradation of the two dyes was observed with TiO2/Ag9.3%, showing optimal kinetics at this doping concentration. The improved photoactivity of the TiO2/Ag composite is due to a decrease in the recombination rate of electron/hole (e−/h+) and a decrease in the band gap from 3.13 to 2.49 eV. The mineralization rate of both dyes under visible light is about 9.3%, indicating the presence of refractory by-products that resist complete degradation. Under UVA irradiation, complete mineralization is obtained. This study confirms the potential of TiO2/Ag composite as a high-performance and cost-effective photocatalyst for solar environmental remediation, highlighting the role of silver in extending light absorption into the visible region and improving charge separation.
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