Under near ambient temperature and ultrasonication, nanocrystalline Zn(Oxin)2·2H2O (zinc 8-quinolinolate) was synthesized by solid state chemical reaction. The particle size distribution was relatively uniform, the morphology of the mare was ball like particle. The phase, particle size and morphology of the prepared nanocrystalline were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM) and electron diffraction (ED). The results show that the crystallite product has an average size of about 30 nm. The effects of a series of reaction conditions on the synthesis of Zn(Oxin)2·2H2O by solid state reaction were studied. During the synthesis of nanocrystalline Zn(Oxin)2·2H2O, the solid state reaction conditions such as changing reactant, matching proportion of reactant, adding inert substance, joining a little solvent or surface active solvent and grinding at different times may influence morphology, particle size and the size distribution of final products. Under near ambient temperature and ultrasonication, nanocrystalline Zn (Oxin) 2 · 2H2O (zinc 8-quinolinolate) was synthesized by solid state chemical reaction. The particle size distribution was relatively uniform, the morphology of the mare was ball like particle. The phase, particle size and morphology of the prepared nanocrystalline were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM) and electron diffraction (ED). The results show that the crystallite product has an average size of about 30 nm. effects of a series of reaction conditions on the synthesis of Zn (Oxin) 2 · 2H2O by solid state reaction were studied. During the synthesis of nanocrystalline Zn (Oxin) 2 · 2H2O, the solid state reaction conditions such as changing reactant, matching proportion of reactant, adding inert substance, joining a little solvent or surface active solvent and grinding at different times may influen morphology, particle size and the size distribution of final pro ducts.