In this study, the polyvinylpyrrolidone (PVP) stabilized Ru and Rh (Ru-Rh@PVP) nanocatalyst was prepared using the precursor materials of Ru, Rh and also PVP as a polymeric material, characterized and its catalytic activity was investigated by using in the hydrolytic dehydrogenation of methylamine-borane (MeAB) at room temperature. The structural and morphological properties of the Ru-Rh@PVP nanocatalyst was examined by using analytical techniques such as TEM/EELS, HRTEM, XPS, P-XRD and UV-Vis spectra. These analytical techniques revealed that Ru-Rh based nanoparticles were well distributed on the PVP with a particle size of 3.42 +/- 0.33 nm. The preparation of catalyst was done according to alcohol reduction technique and then prepared Ru-Rh@PVP nanocatalyst was tested in the hydrolytic dehydrogenation of methylamine-borane at various MeAB-Ru-Rh@PVP concentrations, temperatures and reusability performance at room temperature. The one of the best TOF (initial turnover frequency) and E-a (activation energy) values were found to be 206.2 min(-1) and 43.5 kJ/mol, respectively. (C) 2019 Elsevier B.V. All rights reserved.