An original procedure was applied in order to prepare composite electrocatalysts for hydrogen evolution reaction HER, containing Ni, Co and CoNi as a hyper d – electronic phase and TiO2 as a hypo-phase deposited on conductive carbon substrate Vulcan XC-72. The catalyst’s support (TiO2 and carbon) was thermally treated on 250 and 480°C in the atmosphere of H2 and N2. XRD and SEM methods were employed in order to elucidate the influence of temperature on the structural characteristics of catalysts
