Herein, we report the synthesis of silver-cobalt nanopowders using three different modes of solution combustion synthesis, and we present the effects of the synthesis conditions on particle morphology. The synthesized nanoparticles were characterized using X-ray diffraction (XRD), Scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), UV-Visible spectrophotometer (UV-vis), Transmission electron microscopy (TEM), and X-Ray Photoelectron Spectroscopy (XPS) to understand the structural and elemental properties. When Co is synthesized over Ag in a second wave of combustion, peak shifts observed in XRD and XPS show a change in the cell parameters and prove the existence of a strong electronic interaction between Ag and Co. Better control of mixing and alloying through the second wave combustion synthesis mode (SWCS) was evident. The sequence of combustion affects the structure and composition of the material. SWCS reduces the amount of carbon content, as compared to single-stage combustion, and the combustion of carbon is followed by a rearrangement of atoms.