Crystalline Zn 2 SnO 4 nanoparticles were successfully synthesized via a simple solvothermal route by using Zn(CH 3 COO) 2 ·2H 2 O and SnCl 4 ·5H 2 O as source materials, NaOH as mineralizing agent, and water and ethanol as mixed solvents. The used amount of NaOH was found to have an important influence on the formation of Zn 2 SnO 4 . When the molar ratio of OH − : Zn 2+ : Sn 4+ was set in the range from 4 : 2 : 1 to 8 : 2 : 1, Zn 2 SnO 4 nanoparticles with different shape and size were obtained. However, when the molar ratio of OH − : Zn 2+ : Sn 4+ was set as 10 : 2 : 1, a mixture phase of ZnO and ZnSn(OH) 6 instead of Zn 2 SnO 4 was obtained. Photodegradation measurements indicated that the Zn 2 SnO 4 nanoparticles own better photocatalytic property to depredate methyl orange than the Zn 2 SnO 4 nanopolyhedrons. The superior photocatalytic properties of Zn 2 SnO 4 nanoparticles may be contributed to their small crystal size and high surface area.