2D Sulfur-doped TiSe /Fe O (named as S-TiSe /Fe O ) heterostructures are synthesized successfully based on a facile oil phase process. The Fe O nanoparticles, with an average size of 8 nm, grow uniformly on the surface of S-doped TiSe (named as S-TiSe ) nanoplates (300 nm in diameter and 15 nm in thickness). These heterostructures combine the advantages of both S-TiSe with good electrical conductivity and Fe O with high theoretical Li storage capacity. As demonstrated potential applications for energy storage, the S-TiSe /Fe O heterostructures possess high reversible capacities (707.4 mAh g at 0.1 A g during the 100th cycle), excellent cycling stability (432.3 mAh g after 200 cycles at 5 A g ), and good rate capability (e.g., 301.7 mAh g at 20 A g ) in lithium-ion batteries. As for sodium-ion batteries, the S-TiSe /Fe O heterostructures also maintain reversible capacities of 402.3 mAh g at 0.1 A g after 100 cycles, and a high rate capacity of 203.3 mAh g at 4 A g .