Described is a novel, facile route for the synthesis of nickel supported on hierarchically porous carbon (Ni/HPC) using a one-pot co-gelation sol-gel method. Ni/HPC with varying nickel loadings (0.5,1, 2.5 and 5 wt% Ni) were synthesized and the materials characterized by nitrogen physisorption, X-ray diffraction (XRD), scanning electron microscopy (SEM), and Fourier transform infrared (FTIR) and Raman spectroscopies. The results show a three-dimensional network of disordered carbon with fine nickel nanoparticles of sizes ranging from 8 nm to 13 nm at 0.5 wt% Ni loading which gradually increased with increase in the Ni loading. The carbon structure was retained at the macropore level, but not at the mesoscale where the ordered mesopores were lost on nickel addition. The nickel nanoparticles were observed to grow on the surface of the ligaments. This may make them particularly suitable for low pressure Ni-catalyzed organic transformations e.g., hydrogenations, C-C coupling, C-heteroatom coupling, etc. (C) 2015 Elsevier Ltd. All rights reserved.