In this paper, a method to synthesize anatase TiO2 nanorods by hydrolysis of titanium(IV) isopropoxide (TTIP) in the presence of benzyl alcohol and acetic acid at 210 °C was tested. The novelty of the present approach relies on the evaluation of the shape-controlled synthesis of anatase TiO2 nanocrystals via a microwave-solvothermal method in 45 min. The different TiO2 nanocrystals were obtained by tuning the TTIP/acetic acid ratio under optimized synthetic conditions and were characterized in detail by X-ray diffraction (XRD), transmission electron microscopy (TEM), high-resolution TEM (HRTEM), micro Raman (together with microphotoluminescence) and FT-IR spectroscopies. The acetic acid coordinated on the nanocrystal surface was removed by the reduction of its carboxyl group via a “super-hydride reaction”, and the photocatalytic activity of bare TiO2 nanocrystals, under visible light irradiation, was also …