N-doped TiO2 nanoparticle photocatalysts were prepared through a sol-gel procedure using NH4Cl as the nitrogen source and followed by calcination at certain temperature. Systematic studies for the preparation parameters and their impact on the structure and photocatalytic activity under ultraviolet (UV) and visible light irradiation were carried out. Multiple techniques (XRD, TEM, DRIF, DSC, and XPS) were commanded to characterize the crystal structures and chemical binding of N-doped TiO2. Its photocatalytic activity was examined by the degradation of organic compounds. The catalytic activity of the prepared N-doped TiO2 nanoparticles under visible light (lambda > 400nm) irradiation is evidenced by the decomposition of 4-chlorophenol, showing that nitrogen atoms in the N-doped TiO2 nanoparticle catalyst are responsible for the visible light catalytic activity. The N-doped TiO2 nanoparticle catalyst prepared with this modified route exhibits higher catalytic activity under UV irradiation in contrast to TiO2 without N-doping. It is suggested that the doped nitrogen here is located at the interstitial site of TiO2 lattice.