Highly dispersed bimetallic Ni-Pt nanoparticles with different compositions supported on MIL-101 have been successfully synthesized by a simple liquid impregnation method. The as-synthesized NPs in an average of 1.9 +/- 0.4 nm could be isolated by certification and characterized by using PXRD, TEM, EDX, XPS, BET, and ICP-AES. Catalytic activity of the Ni -Pt@MIL-101 was tested in the hydrogen generation from aqueous alkaline solution of hydrazine. These catalysts were composition dependent for the catalytic activity. Among all the Ni -Pt@MIL-101 catalysts tested, the Ni88Pt12@ MIL-101 exhibited the highest catalytic activity, with the turnover frequency (TOF) value of 350 mol(H2), mol(metal)(-1)h(-1) at 50 degrees C, which is the highest among all the previously reported catalysts. Copyright (C) 2014, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.