In the present work, a new preparation method for metal-polymer composite materials for hydrogen separation which consist of hydride-forming intermetallic compound LaNi5 and polyethylene was developed. According to this technique, the mechanical activation of the initial powder mixtures was employed to provide good interface between the phases. A series of composite membranes with various filler concentrations was synthesized and characterized by X-ray diffraction, scanning electron microscopy and differential scanning calorimetry. The gas transport properties of the obtained materials in relation to H-2, O-2, N-2, CO2 and CH4 were tested. The results indicate that the addition of the hydride-forming intermetallic compound to the barrier polymer leads to significantly improved selectivity with respect to hydrogen. The proposed method can be considered as a promising approach to producing of high performance composite membranes for hydrogen separation. (C) 2018 Hydrogen Energy Publications LLC. Published by Elsevier Ltd. All rights reserved.