Adsorption and encapsulation of the nanoparticles in polyelectrolytes impart stability to the nanometal by preventing aggregation through electrostatic and steric effects. Poly (acrylic acid) (PAA) was employed as a polymer cap to anatase titania nanoparticles. Cross-linking of the polymer was done via free-radical cross-linking using gamma-irradiation. The size of the nanocomposite produced ranged from 40-120 nm. SEM images showed that excess TiO2 in solution becomes nucleation sites for aggregation. Film assembly of the synthesized nanocomposite were done by layer-by-layer deposition with PDDA. Films formed with increasing thickness (5, 10, and 15 layers) were analyzed under AFM and shown to have a thickness of 0.25 μm, 1.1μm and 3.0 μm respectively.The average film layer thickness obtained ranged from 50-200 nm per TiO2/PAA-PDDA layer where as the number of layers deposited increase, the layer thickness increase while the roughness decreases.