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In this study, carbon-coated α-Fe 2 O 3 @Fe 3 O 4 heterostructures were designed and synthesized by a simple ball-milling and an auxiliary rheological phase method combined with carbothermal reduction. Due to the synergistic effect between α-Fe 2 O 3 and Fe 3 O 4 , the carbon-coated α-Fe 2 O 3 @Fe 3 O 4 heterostructures have an excellent electrochemical performance. In order to elucidate the reaction process, the types of gases produced during the pyrolysis of citric acid are preliminarily examined, and the possible chemical reactions are deduced from the experimental results. The Mössbauer spectrum is used to determine the relative ratio of α-Fe 2 O 3 to Fe 3 O 4. As an anode material for lithium ion batteries, a carbon-coated Fe 2 O 3 @Fe 3 O 4 electrode exhibits a high initial discharge/charge capacity of 1462.2/968.2 mAh g−1 and a good reversible capacity (971.5 mAh g−1) at a current density of 0.1 A g−1. Moreover, even after 200 cycles, a reversible capacity of 711.0 mAh g−1 can be maintained at a current density of 0.5 A g−1. • Preparation of carbon-coated Fe 2 O 3 @Fe 3 O 4 heterostructured electrode uses a simple and low-cost method. • The types of reducing gases in the pyrolysis of citric acid were determined and the chemical reaction was inferred. • The possible chemical reaction is deduced from the experiment. • The carbon-coated Fe 2 O 3 @Fe 3 O 4 heterostructured has achieved good rate performance and cycle stability. [ABSTRACT FROM AUTHOR]