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Bimetallic iron/silver (Fe/Ag) core/shell nanoparticles were prepared by chemical reduction from ferrous sulfate in the presence of sodium borohydride as a reducing agent in water, followed then by redox transmetalation with addition of silver nitrate (AgNO3) solution. When the reduction temperature was increased from room temperature to 85 °C, Fe nanoparticles with a reduced crystallite size ranging from 5.5 to 2.0 nm resulted. The particles changed from spherical to plate-like morphology as the temperature reached 85 °C. Addition of trisodium citrate was able to protect the precipitated Fe nanoparticles from oxidation; nonetheless, the citrate would facilitate chelation of the Fe clusters so that dense Fe aggregates with a mean diameter greater than 100 nm were found as the concentration of trisodium citrate exceeded 3.33 mM. A continuous Ag film was formed on the Fe surface by the redox transmetalation. This Ag film became a raspberry structure involving preferential deposition of particulate Ag on the Fe particles when the AgNO3 concentration exceeded 76.9 mM. Magnetic saturation was found to reduce with the increasing Ag concentration in the bimetallic composite nanoparticles.