To improve combustion efficiency and anti-oxidation property of aluminum nanoparticles (ANs), surface nitridation of ANs was performed in a pipe furnace under the protection of nitrogen gas in a glove-operation hermetic box via an off-line nitridation process. The product was characterized by transmission electron microscopy (TEM), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS) analysis. A core-shell nanostructure with an aluminum nitride (AlN) coating on the ANs core was observed. The empirical kinetic triplets (Ea, A, and f(α)) for the nitridation of ANs, for the first time, were calculated and analyzed using five types of iso-conversional methods and a differentiation method. The effects of the kinetics of the reaction were investigated by simultaneous differential scanning calorimetry-thermogravimetry (DSC-TG) and thermal analysis using linear programmed temperature at different heating rates.