Luminescent SiC x N y /AlN nanoparticle superlattices (NPSLs) were fabricated by sputtering SiC and Al targets alternatively under a mixture gaseous flow of N 2 , Ar, and H 2 by plasma RF magnetron sputtering. It was found that the best periodic structures and greatest content of SiC x N y nanoparticles occur in the case in which the sublayer thickness of SiC x N y and AlN are 42 and 3nm, respectively. In this case, the NPSLs exhibit strong photoluminescence (PL) either before or after annealing. Annealing at different temperature (T anneal ) revealed that the PL intensity first increases with increasing T anneal and PL peak is red-shifted when T anneal >650°C; the PL intensity reaches a maximum as T anneal =1100°C. A microstructure model that takes into account the formation energy of SiC x N y nanocrystal limited by AlN sublayers was developed to tentatively explain the formation of SiC x N y nanocrystal in SiC x N y /AlN NPSLs. Based on the structural analysis by X-ray diffraction and Fourier-transform infrared spectra, the PL of SiC x N y /AlN NPSLs was discussed.