Effect of thermal treatments on high surface area anatase TiO₂

Titanium dioxide (TiO₂) is widely employed in catalysis, energy conversion, and environmental applications, where high surface area and crystallinity play crucial roles in enhancing performance. However, achieving thermal stability while maintaining these properties remains challenging. This study investigates the structural and textural evolution of a high-surface-area anatase TiO₂ subjected to various thermal treatments, including vacuum, static, and flow conditions. Through N₂ adsorption, X-ray diffraction, electron microscopy, and in situ infrared spectroscopy, we elucidate the interplay between surface area, crystal growth, surface sites and exposed crystallographic surfaces. Thermal treatments in vacuum preserve the surface area up to 450 °C, while static calcination leads to significant reduction and scarce reproducibility. Controlled flow conditions improve stability, though humidity accelerates sintering. Spectroscopic analyses reveal a strong interaction with water, influencing hydroxylation and dehydroxylation dynamics. Our findings provide insights into optimizing TiO₂ processing conditions for applications requiring high thermal stability and catalytic efficiency.