This study reports on the fabrication and assembly of Ti3C2 MXene and mesoporous NiFe2O4 (m-NiFe2O4) as anode material for Lithium-ion battery (LIB). Here, Ti3C2 MXene was prepared using an etching and exfoliating process. Meanwhile, the mesoporous feature of NiFe2O4 was fabricated via nanocasting method using SBA-15 as a hard template. Based on the result, the integration of the two materials via hydrothermal method was found to demonstrate a synergistic effect in facilitating the migration of Li ions, which resulted in a significant increase in the initial discharge capacity of 1383 mA h g−1 and Coulombic efficiency of 95 %. Such enhancement was believed to have originated not only from the high surface area of m-NiFe2O4 (168.27 m2/g), which was mainly due to its mesoporous feature, but also the unique physicochemical properties and conductivity of Ti3C2 MXene. Besides, theoretical calculation using Density Functional Theory (DFT) also revealed that the adsorption energy of lithium atoms at the composite's surface was found to be more negative than that of individual materials. This suggests that the synergy between the two materials provides a more favorable environment for lithium to be intercalated at the anode, ultimately leading to increased battery performance. © 2025 Elsevier B.V.