ZnSe microspheres were synthesized via a facile hydrothermal method under mild conditions using aqueous zinc nitrate and sodium selenite as raw materials. The effects of hydrothermal temperature, reaction time, concentration of NaOH and amount of hydrazine hydrate on the phase structure, morphology and size of final products were carefully investigated. The phase structures, morphologies and optical properties of the final products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and photoluminescence (PL) spectroscopy. ZnSe microspheres assembled by average size (about 20 nm) nanocrystals were prepared using 20 mL of 1 mol/L NaOH solution and 10 mL of hydrazine hydrate at 180 °C for 4 h. The results show that the products obtained at low hydrothermal temperature and short reaction time have poor crystallinity and contain impurity phases. The appropriate NaOH concentration and amount of hydrazine hydrate ensure to obtain pure ZnSe with spherical morphology and better luminescence property.
The preparation of Zn Se/Cd Se core-shell structure nanocomposites by using the re-prepared Zn Se microspheres as the template under the hydrothermal condition was presented. The influence of different mole ratios of ZnS e to Cd（NO3）2 on the morphology and structure of the final product was investigated. And the performances of ZnS e/Cd Se core-shell structure nanocomposites were characterized by the means of X-ray diffraction（XRD） analyses, scanning electron microscopy（SEM）, transmission electron microscopy（TEM） and photoluminescence（PL） spectroscopy. The results indicate that the core-shell structure product can be prepared, when the mole ratio of Zn Se to Cd（NO3）2 is larger than 1：1; and the product will be ball solid structure, when the mole ratio of Zn Se to Cd（NO3）2 is equal to 1：1. The photo luminescence results show that Zn Se/Cd Se core-shell structures have high photo luminescence emission properties, and the product with mole ratio of Zn Se to Cd（NO3）2 being 1：0.5 has the best luminescence properties.
