In this article, the electrodeposition process of Cu-Sn alloy powders from tripolyphosphate (TPP)-based electrolytes was investigated as a function of deposition parameters. The effects of deposition parameters such as current density, electrolyte composition (Cu/Sn mole ratio), mechanical stirring speed, and temperature on the Cu content of alloy powder and cathodic current efficiency were evaluated using the response surface methodology (RSM). The empirical models developed in terms of deposition parameters were found to be statistically adequate to describe the process responses. The study revealed that as far as the copper content was concerned in the alloyed powders, all parameters selected had positive correlations. However, a high stirring speed and low current density led to a greater current efficiency. The morphology and chemical composition of the electrodeposited Cu-Sn alloy powders were investigated using scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), X-ray diffraction (XRD), and inductively coupled plasma (ICP) analysis. An SEM analysis showed that the powder morphology was affected considerably by the cathodic current density and stirring speed.