In this paper, Fe₂(MoO₄)₃ (FMO) powders have been synthesized via an easy precipitation approach. The microstructural properties of the synthesized product were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS). Two FMO samples, 1 and 2, were synthetized using two reactants, sodium molybdate and ammonium heptamolybdate, respectively. In both cases, pure monoclinic structure with space group P2/a has been identified, via XRD measurements. The crystallite sizes, estimated from Scherer’s formula, are of (38 ± 2) and (46 ± 4) nm according to the precursor used. Besides, the sample 1 showed a relatively larger specific surface area of 42.77 m²/g, than the sample 2 with 35.28 m²/g. The EDS microanalysis confirms the stoichiometric amount of the chemical elements. The SEM micrographs reveal a regular distribution of particles shape that presented grain size of order of (192±52) nm for sample 1. While, the sample 2 presents grains of (215±59) nm size, with a less regular shape.