<p>The exploration of advanced anode materials for lithium-ion batteries (LIBs) has prompted the investigation of NiO/MXene composites, which merge the high theoretical capacity of NiO with the excellent conductivity and structural stability of MXene. This research emphasizes the synthesis, characterization, and electrochemical assessment of NiO/MXene composites as high performance anode materials. Co-precipitation technique is employed to fabricate NiO/MXene material, resulting in a distinct layered structure that alleviates common issues such as volume expansion and particle disintegration during charge–discharge cycles. Structural analyses such as X-ray diffraction and X-ray photoelectron spectroscopy measurements confirms the formation of NiO/MXenes. Morphological examination reveals the even distribution of NiO on MXene surfaces and interlayers. Electrochemical characterization exposed its cycling stability, capacity retention, rate capability and effective capacitive and diffusion contribution. The synergistic interaction between NiO and MXene facilitates lithium-ion diffusion and enhances electronic conductivity. The composite showed a first charge/discharge capacity of 649.47/617.8 mAh g⁻¹ at 0.1C rate, exhibiting significant capacitive and diffusive contribution that supports dual mechanisms of charge storage.</p>