Transition metal dichalcogenides (TMDs) are regarded as the inexpensive and stable electrocatalysts for hydrogen evolution reaction (HER). Designing an electrocatalyst with few-layered molybdenum disulfide (MoS₂) is one of the most effective methods to enhance the activity and durability for HER due to its abundant exposed rim-sites, fast electron transfer and high chemical stability. Herein, a green and facile one-pot approach is developed to synthesize few-layered MoS₂/nitrogen, sulfur codoped porous carbon (MoS₂/NSPC) electrocatalyst via pyrolyzing the in-situ formed molybdate-melamine complex (MoO_x-MEL) within the self-assembled networks of melamine-trithiocyanuric acid (MT). The optimal MoS₂/NSPC electrocatalyst exhibits excellent HER stability and activity with overpotential of 114 mV at 10 mA cm⁻² in 0.5 M H₂SO₄. Furthermore, few-layered tungsten disulfide anchored on N, S-codoped porous carbon (WS₂/NSPC) with high HER activity can also be successfully synthesized by this strategy. It paves a universal way to design active sites–enriched few-layered dichalcogenides with high performance in the applications from energy conversion to storages.

过渡金属二卤化物（TMDs）被认为是用于氢释放反应（HER）的廉价且稳定的电催化剂。设计具有几层二硫化钼（MoS ₂）的电催化剂是增强HER活性和耐久性的最有效方法之一，因为它具有大量暴露的边缘位点，快速的电子转移和高化学稳定性。在此，开发了一种绿色且简便的一锅法，通过热解原位形成的钼酸盐-三聚氰胺络合物（MoO _x -MEL）来合成几层的MoS ₂ /氮，硫共掺杂多孔碳（MoS ₂ / NSPC）电催化剂在三聚氰胺-三硫氰尿酸（MT）的自组装网络中。最佳MoS₂ / NSPC电催化剂在0.5 M H ₂ SO _4中的10 mA cm ^-2下具有114 mV的过电势，具有出色的HER稳定性和活性。此外，通过这种策略，也可以成功地合成几层固定在具有高HER活性的N，S掺杂的多孔碳（WS ₂ / NSPC）上的二硫化钨。它为设计活性位点铺平了一条普遍的途径，即从能量转换到存储的应用中，高性能的，富集的几层二硫属杀菌剂具有高性能。