Recent advancements in zinc-air batteries (ZABs) emphasize the need for efficient and sustainable oxygen electrocatalysts. Central to these efforts are metal-organic frameworks (MOFs), renowned for their bifunctional oxygen electrocatalytic capabilities. However, MOFs and their derivatives often exhibit subpar electrical conductivity and stability. Addressing this, we introduce an innovative approach involving MOFs-derived NiFe2O4/TiO2 nanocrystals sandwiched between 2D MXene nanosheets. This hybrid structure, NiFe2O4/TiO2@NC/Ti3C2, successfully enhances conductivity and active site accessibility, thereby enhancing oxygen reduction (ORR) and evolution (OER) reactions. The NiFe2O4/TiO2@Ti3C2–2 hybrid demonstrates excellent bifunctional activity, characterized by a notable ORR's half-wave potential of 0.846 V and an OER's onset potential of 1.5 V with a potential gap (ΔE) of 0.75 V. When employed in a ZAB, the battery achieves a peak power density of 164 mW cm−2 and maintains cycling stability for over 500 h at 10 mA cm−2. Beyond serving as conductive scaffolds, Ti3C2 MXene nanosheets have a vital role in preserving surface areas of the NiFe2O4/TiO2@NC materials. This study not only highlights a successful strategy for improving oxygen reactions in ZABs but also opens up new opportunities for the development of advanced MOF@MXene catalysts in energy conversion applications.