This paper addresses a new post-treatment strategy for the formation of carbon-encapsulated nickel-cobalt alloys nanoparticles, which is easily controlled the performance of target products via changing precursor composition, calcination conditions (e.g., temperature and atmosphere) and post-treatment condition. Glassy carbon electrode (GCE) modified by the as-obtained carbon-encapsulated mono- and bi-transition metal nanoparticles exhibit excellent electro-catalytic activity for hydrogen production in alkaline water electrolysis. Especially, Ni0.4Co0.6@N-Cs-800-b catalyst prepared at 800 degrees C under an argon flow exhibited the best electrocatalytic performance towards HER. The high HER activity of the Ni0.4Co0.6@N-Cs-800-b modified electrode is related to the appropriate nickel-cobalt metal ratio with high crystallinity, complete and homogeneous carbon layers outside of the nickel-cobalt with high conductivity and the synergistic effect of nickel-cobalt alloys that also accelerate electron transfer process. (C) 2017 Elsevier B.V. All rights reserved.