Addressed herein, the synthesis of the monodisperse poly(3,4-ethylenedioxythiophene)(PEDOT) supported palladiumnickel nanomaterials (3.32 +/- 0.36 nm) and their applications as a catalyst in dimethylamine-borane (DMAB) dehydrogenation is outlined. Microwave assistance procedure was used in preparation of nanomaterials where palladium and cobalt cations were reduced in PEDOT solution (Pd-Ni@PEDOT) in microwave conditions. The characterization of the nanocatalyst was performed by using UV-VIS, XRD, XPS, TEM and HR-TEM-EELS analyses. The Pd-Ni@PEDOT NPs were found to be highly effective and stable for the dehydrogenation of DMAB. The catalytic activity of Pd-Ni@PEDOT was one of the highest one among the all prepared catalysts in literature even at lower temperatures and concentrations, yielding to give high turnover frequency (451.2 h(-1)) and low E-a (50.78 +/- 2 kJ/mol) for dehydrocoupling of DMAB. (C) 2017 Hydrogen Energy Publications LLC. Published by Elsevier Ltd. All rights reserved.