Annealing temperature, a key factor in shaping Ag-decorated TiO2 aerogels as efficient visible-light photocatalysts

Abstract

Ag-decorated TiO₂ aerogels were synthesized using an acid-catalyzed sol–gel method, followed by drying under supercritical CO₂ and annealing within the temperature range of 350–500 °C, with 50 °C increments. This study explores the preparation-structure-performance relationships of

aerogels influenced by the annealing process, focusing on their morphological, (micro)structural, optical, and textural properties and surface defects concerning photocatalytic activity. X-ray diffraction (XRD) and Raman spectroscopy confirmed that all aerogels exhibited a single anatase phase of TiO₂, while electron microscopy (SEM/TEM) and XPS analysis demonstrated the presence of components. Increasing the annealing temperature resulted in particle size and pore structure changes, reducing the aerogel’s overall surface area and porosity, as observed by SEM and nitrogen (N₂) sorption analysis. Additionally, according to the Williamson-Hall (W-H) analysis based on the X-ray peak profile, the lattice microstrain value decreased while the crystallite size increased with rising annealing temperature. Optical investigation showed a strong UV light absorption characteristic of TiO₂ and a visible light absorption band attributed to the plasmonic effect of silver nanoparticles. Moreover, a gradual photoluminescence (PL) quenching trend was observed with decreasing annealing temperature, indicating a reduction in the recombination rate of photo-induced electrons and holes in

, alongside the formation of oxygen vacancies and structural defects, consistent with electron paramagnetic resonance (EPR) measurements. The Ag-decorated TiO₂ aerogels demonstrated enhanced visible-light photocatalytic activity for methylene blue (MB) degradation, with the

aerogel annealed at 500 °C exhibiting the highest photocatalytic performance. This improvement can be attributed to the synergistic effects of chemical composition, plasmonic enhancement, morphological properties, and light absorption characteristics.