Carbon supported Ni@Pt nanoparticles are synthesized using sodium dodecyl sulphate (SDS) and sodium borohydride (NaBH4) as a structure-directing and reducing agents, respectively. The metal loading in synthesized nanocatalyst is 20 wt% and the ratio of Ni:Pt in the nanocatalyst is 1:1. The structural characterizations and morphologies of Ni@Pt/C nanocatalyst are investigated by field emission scanning electron microscopy (FE-SEM), energy-dispersive X-ray spectroscopy (EDX), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HR-TEM) and X-ray diffraction (XRD). The electrocatalytic activity of Ni@Pt/C catalyst toward borohydride (BH4-) oxidation in alkaline medium is studied by means of cyclic voltammetry (CV), chronopotentiometry (CP) and chronoamperometry (CA). The results show that Ni@Pt/C catalyst has superior catalytic activity toward borohydride oxidation (8825.38 mA mg Pt-1). The Membrane Electrode Assembly (MEA) used in fuel cell set-up is fabricated with catalyst-coated membrane (CCM) and catalyst coated gas diffusion medium (CCG) techniques. The effect of two MEA performances on current voltage (I-V) and current power density (I-P) curves in the direct borohydride-hydrogen peroxide fuel cell was investigated using Pt/C 0.5 mg cm(-2) as cathode catalyst and Ni@Pt/C 1 mg cm(-2) as anode catalyst. The influence of cell temperature, sodium borohydride and hydrogen peroxide concentration on the I-V and I-P is determined. The results show that the maximum power density in MEA prepared using CCM method (CCM-MEA) is 68.64 mW cm(-2) at 60 degrees C, 1 M sodium borohydride and 2 M hydrogen peroxide (H2O2) that is higher than MEA prepared using CCG method (CCG-MEA). The impedance results show that with increasing temperature and discharging current, the overall anodic and cathodic charge transfer resistances reduce. (C) 2017 Hydrogen Energy Publications LLC. Published by Elsevier Ltd. All rights reserved.