Mechanical alloying allows obtaining nonequilibrium structures in various systems, often possessing unique properties, including magnetic ones. Considering the unusual structural features of the magnetostrictive Fe-Ga alloy, this approach may be promising for this system. In this work, extensive experimental studies were carried out aimed at studying the features of mechanical alloying of Fe-Ga. The object of the study was the system Fe-20 wt% Ga in which disordered solid solution α-Fe(Ga) is formed. It was shown that high-intensity milling is an effective tool for mechanical alloying of solid-liquid binary system Fe-Ga, but a serious problem is a low powder recovery, less than 50 %. To solve this problem, various process control agents were tested. Their influence on powder recovery, process kinetics, particle size, carbon contamination, and magnetic properties was studied using a large set of techniques such as XRD, SEM, EDS, VSM, LIBS, and others. It has been shown that, based on a combination of factors, the optimal process control agent for this system is ethanol in an amount of 1 wt%