Well-defined hexagonal nanosheets of layered zinc hydroxysulfate (Zn(OH)(2))(3)(center dot)(ZnSO4)(center dot)(H2O)(5) with the side length of 1-20 mu m and thickness of similar to 50 nm has been synthesized by the thermal treatment of ZnSO4-hexamethylenetetramine precursor in water-ethanol mixed solvent at 75 degrees C. The sheet-like morphology was found to closely depend upon the experimental conditions, such as the solvent and the precursor composition. In particular, the products can be easily converted to ZnO nanosheets upon exposing to the irradiation of electron beam. (c) 2005 Elsevier Ltd. All rights reserved.