ZnS nanoparticles and one-dimensional nanocrystals were obtained by in-situ synthesis in Aa-AMPS-hT ternary periodic copolymer by ion complexometry and self-assembly method. The micro-morphology, structure and optical properties were characterized by TEM, SED, UV-vis spectra and PL spectra. The results show that the products are hexagonal ZnS nanocrystals with 15 nm-215 nm in diameter. The morphology and dimension of ZnS nanoparticles could be controlled by varying the sulfuration time. The UV-vis absorption spectra indicate that the absorption edges are blue-shifted by shortening the sulfuration time, exhibiting a marked quantum size effect. With shortening sulfuration time, the photoluminescence emission peak of 409.8 nm is blue-shifted, which could be ascribed to be the forbidden gap emission .