Nitrogen terminated silicon nanoparticles were synthesized on AFI AlPO 4-5 zeolite by pulsed laser ablation of silicon target in the presence of 1.33×10 −5 Pa of ammonia, and were characterized in situ by X-ray photoemission spectroscopy (XPS) and ultraviolet photoelectron spectroscopy (UPS). Nonstoichiometric silicon nitride and unterminated silicon nanoparticles with size of estimated to be ∼5.4 Å in diameter were existed. They were found to migrate and diffuse into the AlPO 4-5 channels at 373 K and migrate back to the external surface at 503 K. The effect of sample annealing was studied at 373 K. The change of silicon surface state (unterminated silicon nanoparticles) to hydride species was observed concurrently with breaking of the NH x species. This result implies that the NH x species remained on the silicon particles form Si 3N 4 like bonds and the dissociated H-species are bound to the unterminated silicon surface.