Layer by layer (LbL) self-assembled technique was used to fabricate TiO 2 films onto glass and quartz slides. The LbL sequence was PAH/PSS/TiO 2 (PSS/TiO 2 ) 5 (PSS=poly(sodium-4-styrene sulfonate), PAH=poly(allylamine hydrocloride)). These LbL thin films were characterized by Raman spectroscopy. The Raman spectrum confirmed the formation of TiO 2 nanoparticles in the anatase phase which average size of the particles around 30nm and thickness of the film estimated around 40nm as determined by atomic force microscopy (AFM). The photodegradation of Congo red (CR) dye immobilized over the LbL film was studied. Reference resonance Raman scattering (RRS) and Raman scattering (RS) spectra of Congo red were recorded with the 514.5nm and 785nm excitation laser lines. The photodegradation experiments were carried out by exposing the LbL TiO 2 film/CR to UV radiation in a container with distilled water. After UV exposure, degradation products were monitored by Raman spectroscopy.