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Lightweight NiAl alloys are expected to replace high-density nickel-based superalloys, but their mechanical performance needs to be improved. In this work, NiAl–30Cr composites with a novel heterogeneous microstructure composed of fine NiAl matrix and Cr single-phase was successfully prepared. Nanoscale Cr particles with 15 nm in size precipitated in NiAl matrix are coherent with NiAl matrix owing to very low interplanar and interatomic spacing mismatch. Such a composite microstructure makes NiAl–30Cr exhibit high strength and high toughness. The yield strength (1207 MPa), ultimate compressive strength (2307 MPa), product of strength and plasticity (29.3 GPa%), and fracture toughness (10.76 MPa m1/2) of NiAl–30Cr increased by 96.6%, 85.6%, 55.1% and 19.7% respectively at room temperature compared to the corresponding ones of NiAl. At 1000 °C, the yield strength (144 MPa) of NiAl–30Cr was 85.9% higher than that of NiAl. Solution strengthening and precipitation strengthening were the key strengthening mechanisms at room temperature. The enhancement in toughness was attributed to grain refinement, increased crack propagation paths, weakened Ni–Al covalent bonding and coordinated deformation of Cr single-phase and NiAl matrix. By contrast, the main strengthening mechanism at 1000 °C is the solid solution Cr atoms hindering dislocation climbing and the stable interface bonding between the Cr nanoprecipitation phase and the NiAl matrix. This work provides new ideas for preparing high-strength and tough NiAl alloy. • NiAl–30Cr consists of NiAl and Cr single-phase, which can coordinate deformation. • Coherent Cr nano-precipitates distribute in NiAl matrix, and interface is stable. • The yield strength increased by 96.6% and 85.9% at 25 °C and 1000 °C. • The strengthening and toughening mechanisms are revealed. [ABSTRACT FROM AUTHOR]