Sn3.5Ag (mass fraction, %) nanoparticles were synthesized by an improved chemical reduction method at room temperature. 1,10-phenanthroline and sodium borohydride were selected as the surfactant and reducing agent, respectively. It was found that no obvious oxidation of the synthesized nanoparticles was traced by X-ray diffraction. In addition, the results show that the density of primary particles decreases with decreasing the addition rate of the reducing agent. Moreover, the slight particle agglomeration and slow secondary particle growth can result in small-sized nanoparticles. Meanwhile, the effect of surfactant concentration on the particle size can effectively be controlled when the reducing agent is added into the precursor at an appropriate rate. In summary, the capping effect caused by the surfactant molecules coordinating with the nanoclusters will restrict the growth of the nanoparticles. The larger the mass ratio of the surfactant to the precursor is, the smaller the particle size is.