Molybdenum sulfide (MoS 2) has emerged as a promising catalyst for hydrogen evolution applications. The synthesis method mainly employed is a conventional hydrothermal method. This method requires a longer time compared to other methods such as microwave synthesis methods. There is a lack of comparison of the two synthesis methods in terms of crystal morphology and its electrochemical activities. In this work, MoS 2 nanosheets are synthesized using both hydrothermal (HT-MoS 2) and advanced microwave methods (MW-MoS 2), their crystal morphology, and catalytical efficiency towards hydrogen evolution reaction (HER) were compared. MoS 2 nanosheet is obtained using microwave-assisted synthesis in a very short time (30 min) compared to the 24 h hydrothermal synthesis method. Both methods produce thin and aggregated nanosheets. However, the nanosheets synthesized by the microwave method have a less crumpled structure and smoother edges compared to the hydrothermal method. The as-prepared nanosheets are tested and used as a catalyst for hydrogen evolution results in nearly similar electrocatalytic performance. Experimental results showed that: HT-MoS 2 displays a current density of 10 mA/cm 2 at overpotential (− 280 mV) compared to MW-MoS 2 which requires− 320 mV to produce a similar current density, suggesting that the HT-MoS 2 more active towards hydrogen evolutions reaction. View Full-Text