Resumen: Bimetallic mesoporous photocatalysts were synthesized via a wet impregnation method using SBA-15 as a support, and characterized by UV–visible diffuse reflectance spectroscopy, low-angle X-ray diffraction and N2 physisorption. Among the tested materials, the Ti/Mn combination exhibited the highest photocatalytic activity in azo dye degradation. To understand this enhanced performance, catalysts with varying Mn loads and calcination ramps were evaluated. Additionally, experiments with radical scavengers (isopropanol, chloroform) and under N2 insufflation were conducted to identify the active radical species. Catalysts prepared with low Mn content and higher calcination ramps showed the greatest activity, which significantly decreased with isopropanol, indicating hydroxyl radicals as the main reactive species. In contrast, samples with higher Mn content and quicker heating displayed reduced activity in the presence of chloroform, suggesting superoxide radical involvement. Spectroscopic analyses (XPS, UV–Vis DRS) revealed that increasing Mn load promotes the formation of Mn2+ over Mn4+ species and lowers the band gap energy. These findings highlight the direct correlation between synthesis parameters, surface composition and optical properties, providing a strategy for fine-tuning the performance of a photocatalyst. Idioma: Inglés DOI: 10.3390/suschem6040031 Año: 2025 Publicado en: Sustainable chemistry 6, 31 (2025), 1-28 ISSN: Financiación: info:eu-repo/grantAgreement/EC/H2020/101007629 /EU/Nanomaterials for Enzymatic Control of Oxidative Stress Toxicity and Free Radical Generation/NESTOR Tipo y forma: Article (Published version) Área (Departamento): Área Física Materia Condensada (Dpto. Física Materia Condensa.)