The highly efficient electromagnetic wave (EMW) absorption materials are considered a promising approach to combatting electromagnetic radiation pollution. We synthesized a novel heterostructure 2D Ti3C2Tx MXene composite film modified by 0D nano-diamond (ND) particles using simple mechanical stirring and a vacuum filtration method. Subsequently, we investigated its microstructure and EMW absorption properties. The ND modification not only regulated the impedance matching of the composite films but also enhanced the diversity of EMW losses, demonstrating excellent microwave absorption performance. With a 40 wt% ND content, the minimum reflection loss (RLmin) of the films reached −43.0 dB, corresponding to a film thickness of 2.5 mm. This study explored a novel and promising microwave absorption film, expanding the application of diamond in microwave absorption, and addressing the theoretical gap in diamond-enhanced MXene microwave absorption performance.