This book explains the major experimental finding on synthesis, characterization and photocatalytic activity of TiO2 based 1-D nanocomposite materials for highly efficient hydrogen (H2) production under solar light irradiation. A simple and effective hydrothermal method was adopted for synthesis of one-dimensional nanostructure such as nanotubes and nanorods. Calcination and impregnation techniques were adopted to improve the crystallinity of pristine titanates and deposition of narrow band gap metal oxides such as Ag2O, CuO and Cu2O on the surface of TiO2 nanostructures. The surface and structural properties of photocatalysts were studied using various characterization techniques. Experimental conditions such as morphologies of catalyst, crystal phase composition, surface chemical composition, amount of catalyst in suspension, water splitting reaction with or without organic scavengers were optimized to achieve the best rate of H2 production. The present study also applicable to bio-mass derived glycerol as sacrificial agent in photocatalytic H2 production paves the sustainable way to dispose-off industrial waste into H2 fuel.