Microwave-assisted hydrothermal synthesis of aluminum (Al)-doped TiO 2 (ALT) and niobium (Nb)-doped TiO 2 (NBT) nanoparticles were carried out. Investigations were performed to examine the crystallinity, vibrational modes, surface morphology, and composition using X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), and energy-dispersive spectroscopy (EDS), respectively. The XRD study indicated the higher crystallinity of the ALT particles compared to the Al and Nb-doped TiO 2 (ALNBT) particles, and only the presence of the anatase phase was observed in all samples. As a result of doping, the Raman mode at ∼147 cm −1 is found to be shifted toward a higher wavenumber for both samples. SEM analysis showed the spherical morphology of ALT and NBT nanoparticles. The elemental composition peaks of Al, titanium, Nb, and oxygen were noticed by EDS measurements. Furthermore, both prepared nanoparticles were used as photocatalytic materials. The Nb and Al-doped samples showed an improvement in the photocatalysis response in relation to the pure TiO 2 sample, in which Al-doped sample was able to decolorize 100% of rhodamine B in 75 min of analysis.