This article studies the synthesis of bimetallic Fe/Au submicron particles with Ultrasonic Spray Pyrolysis (USP). The combination of Fe oxide particles’ ferromagnetism with Au nanoparticles’ (AuNPs) surface plasmon resonance has gained high interest in biomedical and various other applications. Initial investigations for producing Fe/Au particles with USP were carried out in order to study the particle formation mechanisms. Firstly, three precursor salt solutions (Fe acetate, Fe nitrate and Fe chloride) were used to produce Fe oxide particles and to study their effect on particle morphology through characterization by Scanning and Transmission Electron Microscopy (SEM and TEM) with Energy Dispersive X-ray spectroscopy (EDX). These precursor salts produce three types of submicron particles, a mesh of primary nanoparticles, spherical particles and irregular particles, respectively. Next, different solution combinations of precursor salts of Fe and Au were used with the USP. The obtained particles were characterized, and similarities were then examined in the particle formation of pure Fe oxide and Fe/Au particles. The effects of using different salts were analyzed for the formation of favorable morphologies of Fe/Au particles. The combinations of Fe chloride/Au chloride and Fe chloride/Au nitrate in the precursor solution indicate potential in synthesizing bimetallic Fe/Au submicron particles with the USP process.