This study focuses on the preparation of Ni nanoparticle and supports Ni/MgO catalysts by microemulsion assisted synthesis. The study of different synthesis parameters depicted that higher surface area and smaller Ni nanoparticles will be obtained at lower water content due to their small microemulsion droplet size. The addition of MgO support to the microemulsion system leads to a drastic reduction in particle size and provides a protective shell, as depicted by TEM analysis. XRD analysis for pure NiO, MgO, and NiO/MgO reveals the formation of a mild type of NiO-MgO solid solution formation. H2-TPR results indicate lower NiO/MgO catalysts reduction due to the lower free NiO available than pure NiO catalysts. The higher catalytic activity of supported catalysts was dedicated to its higher surface, smaller particle size, and a strong metalsupport interaction than Ni nanoparticles. This study opened up avenues for scholars for further investigations in similar domains.

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