The average size of the TiO₂ nanoparticles was controlled at around 30 nm on Starbon 800 without using any surfactant, which is attributed to the hydrolysis and condensation (it is also proposed to be a plausible condensation with the carboxylate groups on the carbon surface) of the dissolved titanium(IV) isopropoxide into TiO₂ by ultrasonic waves. As the Starbon in the composites has very good contact with the TiO₂ nanoparticles (there is no Ti leaching after 240 min of photocatalysis, XRF analysis) it enhances the photo-electron conversion (better than Norit and graphene oxide carbons) of TiO₂ by reducing the recombination of photo-generated electron–hole pairs. We have prepared an excellent new hybrid photocatalyst for aqueous phase phenol total mineralization.