Nitrogen-doped titania nanoparticles were co-prepared by sol-gel and mechanical-alloying method. Raman spectroscopy was used to investigate the microstructure information of the nitrogen-doped titania nanoparticles. Besides, XPS, ESR and UV-vis absorption spectra were also analyzed as supplementary means. At first blue then red shift of 142 cm-1 peak was observed as the annealing temperatures increased. The possible reasons for the shift were discussed.