Here we describe a new route for the synthesis of nanometric Ni particles embedded in a mesoporous silica material with excellent potential for catalytic applications. Mesoporous silica with a surface area in the range of 202-280 m2/g, with narrow pore size distribution and Ni nanoparticles (particles in the range of 3-41 nm) were obtained in a direct process. A different approach was adopted to process such a nanocomposite. This new approach is based on the formation of a polymer with the silicon oxianion and nickel cation chelated to the macromolecule structure and on the control of the pyrolysis step. The CO/CO2 atmosphere resulting from the pyrolysis of the organic material promotes the reduction of the Ni citrate.