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In this paper, Fe-15at.%Nb alloys were produced from high purity Fe (min. 99.8%) and Nb (min. 99.8%) powders via a mechanical alloying process. The effects of different Process Control Agents (i.e., methanol, hexane, and stearic acid) were investigated with powder morphologies, particle size distribution, and phase formation, and were sampled after up to 80 milling hours at 350 rpm. The powder morphologies and particle sizes were evaluated using scanning electron microscopy and laser diffraction analysis, respectively, and phases were identified via X-ray powder diffractometry. The results demonstrate for all conditions that, in the early stages, there was significant particle agglomeration due to the ductile-ductile feature of Fe and Nb powders, and latter an amorphization trend up to 80 milling hours. Methanol was the most efficient Process Control Agent in terms of avoiding cold welding, reducing of agglomeration, particle size distribution, reducing contamination and crystallinity reduction rate.