SUMMARYIn this study, a two-step process involving a sol-gel and microwave-assisted hydrothermal (MH) techniques has been used to synthesize a novel TiO 2 structure, namely, TiO 2 mesoporous beads. Various hydrothermal synthesis parameters were investigated to study their effects on the resulting beads. It was found that within the processing conditions used, the TiO 2 beads have similar sizes (~325 nm) and contain uniform-sized anatase TiO 2 nanoparticles (<10 nm), which are single crystals. Crystalline TiO 2 beads are obtained in as short as 15 min at a low temperature of only 140°C without any postprocess calcination. Less surface oxygen vacancies was obtained at a higher MH temperature. Compare to the commercial P-25 TiO 2 powders and conventional hydrothermal synthesized TiO 2 beads, MH synthesized TiO 2 beads exhibit much higher values of specific surface areas, pore volumes, and porosities. The use of TiO 2 beads as photocatalyst and photoelectrode for dye-sensitized solar cells has also been investigated.