Metal-oxide nanoparticles can be used to optimize UV absorption and to enhance the stiffness, toughness, and probably the service life of polymeric materials. Characterization of the nano- and microstructure dispersion of particles is necessary to optimize the structure-property relationships. Characterizations of both TiO2 particles dispersed in an acrylic-urethane matrix and TiO2 nanostructured films obtained through sol-gel synthesis are discussed. Experimental methods include microscopy (confocal, AFM) and small angle neutron scattering (SANS). Results from SANS experiments, which yield information about the cluster size of the nano-TiO2 particles and the spatial dispersion in various nanoparticle/polymer samples are presented and compared to the results of microscopy studies.