NiMo and FeMo nanometric particles were prepared by thermal decomposition of water in oil emulsions, where the aqueous phase was a solution of iron or nickel heteropolymolybdates. Decomposition experiments were carried out at 573 K and 70 Bar of hydrogen, with carbon disulfide added to the emulsions. Solids were characterized by X ray diffraction, confocal microscopy and BET surface area. Thiophene hydrodesulfurization was performed in a continuous flow microreactor at 553 K and 1.0 Bar. Particles with diameters between 370 and 560 nm were obtained, and thiophene HDS was in the order NiMoS > MoS approximate to FeMoS > NiS > FeS. The feasibility of using thermal decomposition of emulsions to obtain nanometric bimetallic sulfides particles was shown.