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application/pdf, Nanocrystalline particles of ZnS:(Ag, Al) semiconductor phosphor, whose sizes are mostly 3–5 nm in diameter, are prepared by the gas-evaporation method with cw CO2 laser heating. The Raman scattering spectrum as well as the transmission electron microscope observation demonstrates that the crystallization of the nanoparticles was caused successfully through the gas-phase condensation. Under irradiation of ultraviolet light, the nanoparticles exhibit blue luminescence, as in the case of the starting material of ZnS:(Ag, Al) bulk powder. The peak of the luminescence spectrum of the nanoparticles shifts to lower energy with increasing delay time and also with decreasing excitation intensity, showing that the luminescence originates from the donor–acceptor pair recombination. However, it is concluded that the luminescence of the nanoparticles is not ascribed to the blue Ag luminescence mechanism responsible for the luminescence of the bulk powder, by taking into account the spatial confinement of an electron trapped at the donor and a hole at the acceptor. It is argued that the luminescence mechanism of the nanoparticles is the so called self-activated luminescence, which involves zinc vacancies.