A series of bi-metallic oxygen reduction catalysts derived from pyrolyzed Fe–M (where M=Co, Cu, Ni and Mn) and 4-aminoantipyrine (Fe–M–AAPyr) compounds were prepared using a sacrificial support method (SSM). The influence of the iron interacting with the second metal on the catalytic activity of the oxygen reduction reaction (ORR) was investigated by adjusting the ratio (Fe–M) from 1:3, to 1:1 and 3:1. This series of materials was analyzed and characterized by scanning electron microscopy (SEM) and the BET method (BET) in order to establish structural morphology, and rotating ring disk electrode (RRDE) experiments were performed to evaluate catalytic activity. The results were then correlated to one another, thereby establishing a composition to function relationship. Data from the ring current was used to execute a mechanistic study of the materials for the ORR, and it was found that supplementation of iron with a second transition metal significantly improved catalytic activity.