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Abstract The effect of nitridation treatment on the band alignment between few-layer MoS2 and HfO2 has been investigated by X-ray photoelectron spectroscopy. The valence (conduction) band offsets of MoS2/HfO2 with and without nitridation treatment were determined to be 2.09 ± 0.1 (2.41 ± 0.1) and 2.34 ± 0.1 (2.16 ± 0.1) eV, respectively. The tunable band alignment could be attributed to the Mo-N bonding formation and surface band bending for HfO2 triggered by nitridation. This study on the energy band engineering of MoS2/HfO2 heterojunctions may also be extended to other high-k dielectrics for integrating with two-dimensional materials to design and optimize their electronic devices.