A single-source precursor route is presented to prepare smallsized Ni particles (∼ 5 nm) uniformly embedded into SiO 2 sheet (Ni/SiO 2). The synthetic process involved the coordination of APTES (3-aminopropyltriethoxysilane) with Ni 2 + to form NiÀ Si precursor in high yield, followed by pyrolysis under NH 3 atmosphere. During the heating, the Si component in the NiÀ Si precursor was transformed into SiO 2 , which could restrict the in-situ generated Ni from aggregation, resulting in the formation of the small-sized Ni particles. Small size is conducive to promoting the catalytic performance, and meanwhile SiO 2 protection plays a vital role in improving stability. During aromatic nitro reduction, Ni/SiO 2 shows excellent catalytic performance, which can be separated conveniently by an external magnet after use. The route is indicative of designing other catalysts protected by SiO 2 due to the versatile coordination ability of APTES with other metal ions (Fe, Co, Cu, etc).