A composite of Mo(2)C nanoparticles dispersed onto a nitrogen and sulfur co-doped carbon scaffold (Mo(2)C/N,S-C) was prepared by a simple and environmentally friendly method of one-pot annealing of MoCl(5), urea, and lignosulfonate under a N(2) atmosphere at 700 degrees C. Lignosulfonate, a by-product of the sulfite pulping process, was employed as a feedstock to fabricate the S-doped carbon scaffold and carbide simultaneously, and urea acted as a nitrogen source for N-doping to carbon. The as-prepared Mo(2)C/N,S-C catalyst showed high performance for the hydrogen evolution reaction (HER), with a small overpotential of 105 mV at 10 mAcm(-2), and good stability for 3000 cycles. The improved HER performance of the Mo(2)C/N,S-C originated from the interplay between the highly active Mo(2)C nanoparticles and the N,S co-doped carbon scaffold with its high electrical conductivity and large surface area. Furthermore, N,S co-doping to carbon improved the hydrophilicity of the catalyst surface, thus further enhancing the HER activity.