Abstract: Using ZnSO4·7H2O and Na2SnO3·3H2O as raw materials，ammonia as soft templates，and β-cyclodextrin（CD） controlling the morphology，zinc hydroxystannate［ZnSn（OH）6］microspheres were prepared at room temperature.The effects of the dosage of β-CD，the amount-of-substance ratio of the reactants，and the reactant concentration etc.on the product′s morphology were discussed.The optimum reaction conditions were as follows: the dosage of β-CD was 9 g/L，the amount-of-substance ratio of the reactants was n（Zn2+）∶n（SnO32-）=2∶3，and the reactant concentration was 0.3 mol/L.The products prepared were characterized and analyzed by X-ray diffraction（XRD），scanning electron microscope（SEM），and thermal analysis（TG-DTA）. Moreover，the reaction mechanism was also investigated.

Key words: zinc hydroxystannate；microspheres；&beta, -cyclodextrin