The Ni-Mo + PTh layers were prepared by electrodeposition from a bath containing Ni2+, MoO42-, ClO4- ions and thiophene (Th) The process was conducted in galvanostatic conditions. Surface morphology was examined using scanning electron microscope The steady-state polarization and electrochemical impedance spectroscopy (EIS) methods were used for characterization of electrochemical activity during hydrogen evolution Based on the obtained results parameters of hydrogen evolution process have been determined. It Was found that the process proceeds better on the coatings containing an embedded 4.6% PTh than on the Ni-Mo layers Kinetic parameters of hydrogen evolution are better for the Ni-Mo + PTh layers for comparable Ni-Mo alloy. (c) 2009 Elsevier B.V. All rights reserved