In this paper, TiO₂ prepared with an aqueous sol-gel synthesis by peptization process is doped with nitrogen precursor to extend its activity towards the visible region. Three N-precursors are used: urea, ethylenediamine and triethylamine. Different molar N/Ti ratios are tested and the synthesis is adapted for each dopant. For urea- and trimethylamine-doped samples, anatase-brookite TiO₂ nanoparticles of 6–8 nm are formed, with a specific surface area between 200 and 275 m²·g⁻¹. In ethylenediamine-doped samples, the formation of rutile phase is observed, and TiO₂ nanoparticles of 6–8 nm with a specific surface area between 185 and 240 m²·g⁻¹ are obtained. X-ray photoelectron spectroscopy (XPS) and diffuse reflectance measurements show the incorporation of nitrogen in TiO₂ materials through Ti–O–N bonds allowing light absorption in the visible region. Photocatalytic tests on the remediation of water polluted with p-nitrophenol show a marked improvement for all doped catalysts under visible light. The optimum doping, taking into account cost, activity and ease of synthesis, is up-scaled to a volume of 5 L and compared to commercial Degussa P25 material. This up-scaled sample shows similar properties compared to the lab-scale sample, i.e., a photoactivity 4 times higher than commercial P25.

This work reviews an eco-friendly process for producing TiO₂ via colloidal aqueous sol–gel synthesis, resulting in crystalline materials without a calcination step. Three types of colloidal aqueous TiO₂ are reviewed: the as-synthesized type obtained directly after synthesis, without any specific treatment; the calcined, obtained after a subsequent calcination step; and the hydrothermal, obtained after a specific autoclave treatment. This eco-friendly process is based on the hydrolysis of a Ti precursor in excess of water, followed by the peptization of the precipitated TiO₂. Compared to classical TiO₂ synthesis, this method results in crystalline TiO₂ nanoparticles without any thermal treatment and uses only small amounts of organic chemicals. Depending on the synthesis parameters, the three crystalline phases of TiO₂ (anatase, brookite, and rutile) can be obtained. The morphology of the nanoparticles can also be tailored by the synthesis parameters. The most important parameter is the peptizing agent. Indeed, depending on its acidic or basic character and also on its amount, it can modulate the crystallinity and morphology of TiO₂. Colloidal aqueous TiO₂ photocatalysts are mainly being used in various photocatalytic reactions for organic pollutant degradation. The as-synthesized materials seem to have equivalent photocatalytic efficiency to the photocatalysts post-treated with thermal treatments and the commercial Evonik Aeroxide P25, which is produced by a high-temperature process. Indeed, as-prepared, the TiO₂ photocatalysts present a high specific surface area and crystalline phases. Emerging applications are also referenced, such as elaborating catalysts for fuel cells, nanocomposite drug delivery systems, or the inkjet printing of microstructures. Only a few works have explored these new properties, giving a lot of potential avenues for studying this eco-friendly TiO₂ synthesis method for innovative implementations.