Abstract Tuning heterointerfaces between hybrid phases is a very promising strategy for designing advanced energy storage materials. Herein, a low‐cost, high‐yield, and scalable two‐step approach is reported to prepare a new type of hybrid material containing MoS 2 /graphene nanosheets prepared from ball‐milling and exfoliation of commercial bulky MoS 2 and graphite. When tested as an anode material for a sodium‐ion battery, the as‐prepared MoS 2 /graphene nanosheets exhibit remarkably high rate capability (284 mA h g −1 at 20 A g −1 (≈30C) and 201 mA h g −1 at 50 A g −1 (≈75C)) and excellent cycling stability (capacity retention of 95% after 250 cycles at 0.3 A g −1 ). Detailed experimental measurements and density functional theory calculation reveal that the functional groups in 2D MoS 2 /graphene heterostructures can be well tuned. The impressive rate capacity of the as‐prepared MoS 2 /graphene hybrids should be attributed to the heterostructures with a low degree of defects and residual oxygen containing groups in graphene, which subsequently improve the electronic conductivity of graphene and decrease the Na + diffusion barrier at the MoS 2 /graphene interfaces in comparison with the acid treated one.

MoS 2 /Graphene Nanosheets from Commercial Bulky MoS 2 and Graphite as Anode Materials for High Rate Sodium‐Ion Batteries