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Sb2O3 nanoparticles are uniformly anchored on reduced graphene oxide (rGO) sheets via a facile and ecofriendly route based on the alcohol dissolution–reprecipitation method. Such obtained Sb2O3/rGO composite demonstrates a highly reversible specific capacity (1355 mA h g–1 at 100 mA g–1), good rate capability, and superior life cycle (525 mA h g–1 after 700 cycles at 600 mA g–1) when used an anode electrode for lithium-ion batteries (LIBs). The outstanding electrochemical properties of Sb2O3/rGO composite could be attributed to its unique structure in which the strong electronic coupling effect between Sb2O3 and rGO leads to an enhanced electronic conductivity, structure stability, and electrochemical activity during reversible conversion-alloying reactions. Also, these findings are helpful in both developing novel high-performance electrodes for LIBs and synthesizing functional materials in an ecofriendly and economical way.