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Incorporating dopants into the TiO 2 single crystals lattice is a big challenge because single crystal has a high crystallinity and the nucleation and growth of TiO 2 single crystals is readily subjected to the interference of the dose of dopant precursors. Here, we propose an in situ synthetic strategy for the construct of carbon-doped TiO 2 single crystal nanorods using CPS/TiO 2 as the precursors of TiO 2 nanorods and carbon source via a facile hydrothermal route. This technique involves the preparation of cationic polystyrene spheres (CPS), sequential deposition of TiO 2 precursor, hydrothermal reaction, and the pyrolysis of CPS in a N 2 atmosphere at 450 °C. The morphology and structure of as-prepared C-TiO 2 single crystal nanorods were characterized by TEM, SEM, STEM Mapping, XRD, UV–vis spectroscopy, and XPS. All results confirm the carbon doping in the as-prepared TiO 2 single crystal nanorods. As a result of unique microstructure, the resulting TiO 2 exhibits remarkably visible-light photocatalytic efficiency for the degradation of organic pollutants including methylene blue (MB), Rhodamine B (RhB) and p -nitrophenol (PNP). Therefore, the current study provides a new insight for incorporating dopants into the TiO 2 single crystals lattice. [ABSTRACT FROM AUTHOR]