The current research work focuses on the synthesis of a novel nano-structured porous nickel alloy based composite material with a high catalytic activity for the hydrogen separation application. The revealed composite through this study is a metallic nickel-boron based catalyst supported by nylon fiber. The preparation procedures of this composite had started by loading the nickel alloy particles on the fabrics of the template. This was executed via a special technique of the electroless plating (ELP). This technique differs fundamentally from the ELP impregnation systems since the porosity of the obtained composite is reduced as a result of the compaction during the procedures of the metal particles deposition. Furthermore, the mechanism of depositing the metal particles within the pores of the template, as provided in this technique, is novel. The nano-sized metallic structure of the catalyst was subsequently obtained via a high temperature thermal treatment step. The produced nickel-alloy composite was then applied in the separation of hydrogen from binary mixtures composed of different ratios of hydrogen to nitrogen. A non-typical separation technique is introduced through this research study. Specifically, a combination between the concepts of the cross flow membrane separation and pressure swing adsorption (PSA) techniques is presented. The performance of the prepared composite was evaluated, in terms of the acquired hydrogen recovery. Promising results were demonstrated at the end of this investigation since a significant catalytic separation activity was detected. The structural and morphological properties of the nickel based material were characterized by both scanning electron microscopy (SEM) and X-ray diffraction (XRD). (C) 2016 Elsevier B.V. All rights reserved.