Nanobinary (Mg-Al) and ternary (Ni-Mg-Al) metal oxy/hydroxides were synthesized by aerogel protocol. The key features of this method are homogenization of metal organic precursors in methanoltoluene mixture, controlled hydrolysis, gelation, hydrothermal treatment, and finally supercritical drying of solvent. The obtained materials, which on further drying at 120 degrees C, display high surface area, > 500 m(2) g(-1), and smaller particle size, < 20 nm. The samples were further characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), thermogravimetric and differential thermal analysis (TG-DTA), and solid state Al-27 nuclear magnetic resonance (NMR). The ion exchange and catalytic properties of the resulting nanomaterials were compared with hydrotalcite-like layered double hydroxides (LDHs) prepared by a conventional coprecipitation method. The nanoternary system exhibits 2-4-fold increase in activity of pre-reforming of naphtha.