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Mo sulfide thin films were cathodically electrodeposited onto glassy carbon electrodes (GCE) from aqueous electrolytes containing 10 mM (NH 4) 2 MoS 4 and 0.2 M KCl. Film adhesion was adequate only for electrodes pretreated by potential cycling in 1.0 M HNO 3 and 0.1 M NaF to enhance the surface roughness and partially oxidize the GCE. Previous studies report direct cathodic electrodeposition of MoS 2 , but energy dispersive x-ray spectroscopy and x-ray diffraction suggest that the as-deposited film is closer in stoichiometry to MoS 3 , which can be converted to MoS 2 by annealing in Ar at 600°C for one hour. The charge storage capability of electrodeposited Mo sulfide films is studied here for the first time in 1.0 M Na 2 SO 4 over the thickness range 50 nm to 5 µm, and before and after high temperature annealing. The highest