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Bimetallic catalysts with alloy structure have been extensively explored to tailor and boost the catalytic performance of the dry reforming of methane. Herein, NiFe/Al 2 O 3 catalyst was designed from an aluminum gel with metal nitrate in a triblock copolymer solution by an evaporation-induced self-assembly process and calcination for the low-temperature dry reforming of methane (LT-DRM). The resultant NiFe/Al 2 O 3 exhibited a large surface area of 203 m 2 g −1 and porosity of 0.8 cm 3 g −1 . Bimetallic NiFe/Al 2 O 3 promoted CH 4 and CO 2 conversion as well as the H 2 / CO ratio relative to monometallic Ni/Al 2 O 3 . CH 4 and CO 2 conversion on the NiFe/Al 2 O 3 was 26.6 and 37.8% with a H 2 / CO ratio of 0.67 at 550 °C. Furthermore, NiFe/Al 2 O 3 possessed good stability at 450 °C during LT-DRM reaction for 20 h. The Ni 3 Fe alloy structure is favorable for the resistance of oxidation and coke deposition. This work sheds light on the sophisticated design of the alloy structure of the bimetallic catalyst for efficient and stable catalytic performances.