As an electrocatalyst with abundant resources and great potential, molybdenum disulfide is regarded as one of the most likely alternatives to expensive noble‐metals catalysts. However, it is still a challenge to achieve large scale production of few‐layer MoS₂ with enhancing activity of electrocatalytic hydrogen reaction at ambient conditions. Herein, we developed a simple environmentally friendly two‐step method, which included intercalation reaction and a subsequent electrochemical reduction reaction for mass preparation of defect‐rich desulfurized MoS_x (D−MoS_x ) nanosheets with plentiful sulfur vacancies. The ratio of sulfur‐molybdenum atoms can be adjusted from 2 : 1 to 1.4 : 1 by regulating the desulfurization voltage. It was found that the HER catalytic activity of the D−MoS_x was enhanced compared with that of pristine MoS₂ (P−MoS₂), the current density of D−MoS_x (desulfurization at −1.0 V) at −0.3 V versus RHE was about 169% of the P−MoS₂, and the Tafel slope decreased to 136 mV dec⁻¹. This method can be widely applied to large‐scale preparation of other two‐dimensional materials.

中文翻译：

---

在温和条件下制备的用于增强电催化氢释放反应的大规模二维MoSx催化剂。

作为具有丰富资源和巨大潜力的电催化剂，二硫化钼被认为是昂贵的贵金属催化剂最有可能的替代品之一。然而，在环境条件下实现具有增强的电催化氢反应活性的大规模生产少量MoS ₂仍然是一个挑战。本文中，我们开发了一种简单的环保两步法，其中包括插层反应和随后的电化学还原反应，用于大量制备富缺陷脱硫MoS _x（D-MoS _x）具有大量硫空位的纳米片。通过调节脱硫电压，可以将硫钼原子的比例从2：1调整为1.4：1。发现与原始MoS ₂（P-MoS ₂）相比，D-MoS _x的HER催化活性得到了增强，D-MoS _x（-1.0 V时的脱硫）在-0.3 V时的电流密度与RHE约为P-MoS _2的169％，Tafel斜率降至136 mV dec ^-1。该方法可广泛应用于其他二维材料的大规模制备。