Mo sulfide thin films were cathodically electrodeposited onto glassy carbon electrodes (GCE) from aqueous electrolytes containing 10 mM (NH4)2MoS4 and 0.2 M KCl. Film adhesion was adequate only for electrodes pretreated by potential cycling in 1.0 M HNO3 and 0.1 M NaF to enhance the surface roughness and partially oxidize the GCE. Previous studies report direct cathodic electrodeposition of MoS2, but energy dispersive x-ray spectroscopy and x-ray diffraction suggest that the as-deposited film is closer in stoichiometry to MoS3, which can be converted to MoS2 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 Na2SO4 over the thickness range 50 nm to 5 µm, and before and after high temperature annealing. The highest capacitance is obtained for 50 nm thick MoS2 films is 330 F/g measured by galvanostatic charge discharge at 0.75 A/g, and 360 F/g measured by cyclic voltammetry at 10 mV/sec. The capacitance per unit mass decreases with increasing film thickness due to reduced electrochemical accessibility. MoS2 film formed by high temperature annealing in Ar have a charge storage capability about 40x higher than the as-deposited Mo sulfide films.
Falola, Daniel, Wiltowski, Tomasz and Suni, Ian. "Electrodeposition of MoS2 for Charge Storage in Electrochemical Supercapacitors." Journal of the Electrochemical Society 163, No. 9 (Jan 2016): D568-D574. doi:10.1149/2.0011610jes.