Nano-hybrid materials of anatase and activated carbon were fabricated in a single step by a hydrothermal with ball milling method (H with B) using a conventional autoclave and SiC balls at 180°C. To investigate the influence of ball milling and activated carbon, a hydrothermal method without ball milling (H without B) and a carbonless hydrothermal method with ball milling (Carbonless H with B) were performed. By comparing the three samples based on Transmission Electron Microscopy (TEM) observation and Selected Area Electron Diffraction (SAED) analysis, it was revealed that TiO2 particles in the hybrid materials heterogeneously nucleate on the activated carbon and have a tendency of crystal growth along the c axis under the given experimental condition. The crystal growth direction was controlled isotropically by assisting the ball milling during reaction. The balls seem to act as a stirrer rather than a grinder for the sample containing the activated carbon.