Abstract: The present work relates to the manufacture of the Ni/Al2O3 catalyst and is particularly directed towards the preparation of nano-metallic nickel supported on an alumina catalyst through a novel method that permits the nickel and alumina to be derived from aluminium and nickel nitrates as the source of aluminium and nickel particles. In a broad embodiment, this article relates to preparing Ni/Al2O3 nanoparticles using a glycine-assisted combustion method with simple and inexpensive procedures. In the present specification and appended claims of this invention, it avoids both nickel-metal oxidation and metal-support interaction yielding nickel aluminates as undesired materials. This is achieved by adjusting the ratio between fuel and oxidizers (F/O) at 2. The results revealed that the as-prepared catalysts consisted of Ni and Al2O3 with particle sizes ranging from 6-15 and 3-6 nm, respectively. The as-synthesized particles are regular in shape and have a porous and spongy network structure.