We report the synthesis of a spectrum of highly crystalline molybdenum sulphide/oxide-based materials such as MoS 2 (2-H), MoO 2 and unique hybrid MoS 2 /MoO 2 nanostructures through chemical vapour deposition (CVD). The as-fabricated samples were scrutinized with materials characterization techniques. Our results reveal that, by tuning growth parameters, different samples demonstrate unique morphologies, which can be unequivocally tied to their chemical composition. We also explore their potential application as electrochemical catalysts, which we found that in addition to using large specific surface area and conductive substrate to improve interlayer conductivity,chemical heterogeneity and efficient charge transport are also essential for good catalytic activity. IMPACT STATEMENT We successfully fabricated an array of uniquely shaped MoS 2 /MoO 2 nanostructures through a one-step chemical vapour deposition process. The practical application of said nanostructures as electrochemical catalysts has also been demonstrated.