TiO2 nanoparticles have been prepared by amine template-assisted sol-gel precipitation and further hydrothermal treatment. We have investigated the effect of different amines (hydrazine and triethylamine) in the final surface and structural properties. It has been stated that the different amounts of amine could act as an interesting template upon hydrothermal treatment. Further thermal treatment also leads to a significant improvement in the photocatalytic properties of the studied systems. Surface and morphological features notably differ from TiO2 prepared using different synthetic routes. Wide surface and structural characterization of the samples have been carried out, and correlations with precipitation pH are pointed out from this characterization. In all cases, amine template TiO2 obtained exhibit high conversion values for phenol photo-oxidation reaction. Further calcination treatment of all the studied systems clearly leads to photocatalytic conversions higher than that exhibited by TiO2 Degussa P25. (C) 2007 Elsevier B.V. All rights reserved.