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Abstract The synergistic effects of surface treatment and interleaf on the interlaminar mechanical properties of glass fiber-aluminum laminates were studied. Aluminum sheets were treated with alkaline etching. Meanwhile, a graphene oxide (GO) interleaf was introduced between the aluminum sheet and the glass fiber-reinforced epoxy composite. Double cantilever beam and end-notched flexure tests were employed to evaluate the interlaminar fracture toughness of the glass fiber-aluminum laminates. The obtained results show that the toughening efficiency of the interleaf is dependent on the aluminum surface characteristics as well as the GO loading. Further comparison reveals that the highest mode-I and mode-II fracture toughnesses are obtained in the specimens with alkali etching treatment and addition of GO interleaf with 0.5 wt% of GO loading, which are 510% and 381% higher in comparison to the plain specimen. Fracture surfaces were observed to further uncover the reinforcement mechanisms.