Abstract Polliwog-like Sn/Zn 2 SnO 4 (P-Sn/ZTO) heterostructures have been fabricated by reducing cube-like ZnSnO 3 nanoparticles in the mixed solvent of oleic acid (OA) and 1-octylamine. Energy-dispersive X-ray spectrometry indicates that the stems of P-Sn/ZTO nanostructures are composed by ZTO, and the tips of the P-Sn/ZTO nanostructures are formed by the core of Sn and the shell of ZTO. And the position of Sn can be controlled at the tip of Zn 2 SnO 4 nanowires. Adequate evidences demonstrate that 1-octylamine in the mixed solvent acts as the reducing agent to salt out elementary substance Sn, and the OA plays the important role in controlling the morphology of Zn 2 SnO 4 . In addition, the P-Sn/ZTO structures exhibited excellent gas sensing properties toward ethanol, and the P-Sn/ZTO is a promising potential gas sensing material.