An alkaline solution for the electrodeposition of Fe-Mo alloys was developed with trisodium nitrilotriacetate (NTA(3-)) as the complexing agent for Fe(III). The Fe-Mo voltammetric profile in the presence of 0.11 M NTA and 0.055 M NTA showed, respectively, two cathodic waves and one cathodic wave. Analysis of chemical composition by EDS of electrodeposits produced voltammetrically up to several final electrodeposition potentials (E-f) showed that they contained Fe, Mo and O, depending on E-f. SEM of Fe-Mo electrodeposits with electrodeposition charge density (q(d)) 95.55 C cm(-2), produced potentiostatically with 0.055 M and 0.11 M NTA, showed uniform films formed by coalesced globular crystallites, depending on the deposition potential (E-d). EDS analysis of Fe-Mo electrodeposits produced with q(d) 95.55 C cm(-2) in the presence of 0.11 M NTA showed that the Mo content varied with E-d from 23.3 wt% to 66.2 wt%, whereas in the presence of 0.055 M NTA it varied with E-d from 58.6 wt Mo to 64.4 wt%. XRD analysis of the Fe-Mo electrodeposits produced with q(d) 95.55 C cm(-2), regardless of the NTA concentration, indicated that the Fe-Mo electrodeposits could be of low crystallinity or partially amorphous. (C) 2016 Elsevier B.V. All rights reserved.