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MAX phases represent a crucial building block for the synthesis of MXenes, which constitute an intriguing class of materials with significant application potential. This study investigates the catalytic properties of the Mo 2 TiAlC 2 MAX phase and the corresponding Mo 2 TiC 2 T x MXene for the hydrogen evolution reaction (HER). Characterization by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive spectroscopy (EDS), and X-ray photoelectron spectroscopy (XPS) revealed that despite the presence of secondary phases, the HER catalytic activity is primarily influenced by the MAX phase and its derived MXene. Interestingly, the catalytic activity of the MXene improves over time, attributed to the formation of MoO 2 as identified by XPS. This work enhances the understanding of MXene-based materials for electrochemical applications, highlighting crucial structural and chemical transformations that optimize their performance in energy conversion technologies., Competing Interests: The authors declare no competing financial interest., (© 2024 The Authors. Published by American Chemical Society.)