ZnO, Fe 0.01 ZnO, Sn 0.05 ZnO, and Fe 0.01 Sn 0.01 ZnO photocatalysts are prepared by a simple low-temperature solution method using Zn(NO 3 ) 2 , Fe(NO 3 ) 3 , SnCl 4 , and NaOH as raw materials. X-ray diffraction, field-emission scanning electron microscopy, high-resolution transmission electron microscopy, energy-dispersive X-ray spectroscopy, Brunauer-Emmett-Teller surface area analysis, X-ray photoelectron spectroscopy, ultraviolet-visible diffusion spectroscopy, and photoluminescence spectroscopy are performed to characterize the products. All doped ZnO samples exhibit enhanced photocatalytic activity compared with undoped ZnO toward methylene blue (MB) degradation. In particular, Sn 0.05 ZnO shows excellent performance among the doped samples. The degradation rate of MB by Sn 0.05 ZnO reaches 99.61% after 120 min of illumination, which is approximately 2.2 times as high as that by undoped ZnO (45.88%). A comparison of the photocatalytic activity of the samples reveals the effects of Fe 3þ and Sn 4þ doping on the photocatalytic performance of ZnO on the basis of the following aspects: formation of impurity level, particle size, and pore structure of catalyst, microstructural changes in the crystal, and action of doped ions.