Thin films of azopolymer-nanoparticles hybrid materials were fabricated with poly[1-[4-(3-carboxy-4-hydroxyphenylazo) benzenesulfonamido]-1,2-ethanediyl] (PAZO) and different concentrations of Ag and AgAu nanoparticles (NPs). By illuminating the films with polarized interference patterns, surface relief gratings (SRGs) were recorded. It was found that for some concentrations of NPs their modulations and diffraction efficiency were higher than the obtained for PAZO films without NPs. The effect was mainly explained by the increase of the free volume available for the photoisomerization for certain concentrations of NPs. The dependence of the diffraction efficiency on concentration was directly related to changes in modulation depth. When doping with NPs, the maximum efficiency increases more than two times the efficiency without NPs.