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High crystalline quality wurtzite-GaN nanoparticles, with diameters of about 11 nm, well dispersed in a poly-methyl methacrylate polymer matrix, were synthesized using a routine two-step route and were structurally and optically characterized. The as-prepared composite showed three broad overloading photoluminescence emission peaks with centers at 3.45,3.29, and 3.10 eV. The 3.45 eV emission band is assigned to the recombination of the free exciton of GaN particles. The other two emission peaks possibly originate from the interfacial structure between the nanoparticles and polymer matrix or aggregation. The Fourier transform infrared (FTTR) spectrum further confirms the interfacial interaction that can be described as R-(C=O)-O-(GaN particle).