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To improve the photocatalytic activity of TiO2, a series of NiO–TiO2 nanotubes (NTbs) is prepared by impregnating TiO2 nanotubes in a solution of NiCl2·6H2O at different concentrations. Self-organized TiO2 nanotubes are prepared by a two-step anodization process. Scanning electron microscopy images show that large particle agglomerates are formed for higher precursor concentrations, and X-ray energy-dispersive spectroscopy results indicate that the atomic percentages of Ni in the NiO–TiO2 NTbs prepared with precursor concentrations of 100 and 300 mM are 1.95% and 4.23%, respectively. Electronic lifetime measurements show that the recombination rate of photogenerated electron–hole pairs is lower for NiO–TiO2 NTbs compared to that of TiO2. Specifically, the recombination rate of the sample prepared at 50 mM is the lowest, which is associated with the longest electron lifetime. Compared to unmodified TiO2 nanotubes, NiO–TiO2 NTbs exhibit improved results for the photocatalytic degradation of rhodamine B.