The present work reports on the preparation of NixSy-MoS2 hybrid microspheres (NMSHMs) via one-pot hydrothermal treatment of aqueous solutions of Na2MoO4 center dot 2H(2)O, Ni(NO3)(2)center dot 6H(2)O and H2NCSNH2. As an electrocatalyst toward hydrogen evolution reaction, the NMSHMs exhibit superior activity over MoS2, NixSy and the physical mixture of MoS2 and NixSy in acidic solutions. Such NMSHMs catalyst also shows good durability. (C) 2014 Elsevier Ltd. All rights reserved.