With different mass ratios, titanium dioxide/carbon nanotube (0.1-10 wt% CNTcontent) nanocomposites were prepared with the aid of ultrasonication method. The structures of the various TiO2/CNT nanocomposites were characterized by electron microscopy (scanning electron microscopy, transmission electron microscopy). Their photocatalytic activity was tested by the degradation of phenol in aqueous solution under near-UV irradiation. In parallel experiments, both (SW and MW) CNT samples were treated in a reflux system with nitric acid to functionalize the nanotubes, subsequently preparing the nanocomposites in the same method. At higher CNT concentration (5, 10 wt%) the nanocomposites exhibited lower photocatalytic activity compared to the samples with lower CNT concentration, probably because the higher CNT concentration reduces the light intensity on the surfaces of TiO2 particles. Our aim was to find the best synthesis method and the optimal composition of the TiO2/CNT nanocomposites for the degradation of phenol under UV irradiation. The highest degradation rate was achieved with Aldrich anatase/functionalized single wall carbon nanotube nanocomposite (AA+f-SW1 wt%). The photocatalytic activity of this sample was significantly higher compared to the bare Aldrich anatase and Aeroxide P25 titanium dioxide reference samples which were the best photocatalysts among the investigated bare titanias. (C) 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim