The microstructure of FeAl40 intermetallic alloy produced by spray atomization and deposition, with boron additions and reinforced with Al2O3 particles was studied. This technique allowed the co-deposition of particulate reinforcement and the addition of boron in order to obtain a boron concentration of 0.4 at. %. The additions of alumina particles produce a grain refinement. High resolution transmission electron microscopy observations shows a precipitation of boron in the FeAl matrix in despite of the rapid solidification process. Fe3B precipitates were found which is a metastable phase formed during the rapid solidification process. In addition, FeB precipitates were observed.