Open AccessElectrodeposition of MoS2 from Dichloromethane
Author(s) -
Steve Thomas,
Danielle E. Smith,
Victoria K. Greenacre,
Yasir Noori,
Andrew L. Hector,
C. H. de Groot,
Gillian Reid,
Philip N. Bartlett
Publication year - 2020
Publication title -
journal of the electrochemical society
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.258
H-Index - 271
eISSN - 1945-7111
pISSN - 0013-4651
DOI - 10.1149/1945-7111/ab9c88
Subject(s) - quartz crystal microbalance , amorphous solid , scanning electron microscope , raman spectroscopy , electrochemistry , cyclic voltammetry , materials science , transition metal , inorganic chemistry , annealing (glass) , dichloromethane , chemistry , analytical chemistry (journal) , electrode , chemical engineering , solvent , crystallography , metallurgy , catalysis , biochemistry , physics , adsorption , chromatography , optics , composite material , engineering , organic chemistry
The electrodeposition of MoS 2 from dichloromethane (CH 2 Cl 2 ) using tetrabutylammonium tetrathiomolybdate ([N n Bu 4 ] 2 [MoS 4 ]) as a single source precursor is presented. The electrodeposition of MoS 2 from CH 2 Cl 2 requires addition of a proton donor to the electrolyte and trimethylammonium chloride (Me 3 NHCl) was used for this purpose. Electrochemical Quartz Crystal Microbalance (EQCM) experiments have been employed for a detailed study of the electrochemical mechanism and to study the role of the proton donor. EQCM reveals cathodic electrodeposition of MoS 2 and anodic deposition of MoS 3 as well as an additional corrosion process where the deposited MoS 3 strips back into solution. The electrodeposited MoS 2 films are amorphous in nature. All the films were found to be homogeneous in composition across the electrode area and to be reproducible between experiments. Annealing of the as-deposited films under a sulfur atmosphere results in crystalline MoS 2 as confirmed by energy dispersive X-ray spectroscopy (EDX), Raman spectroscopy and X-ray diffraction. The deposited films were smooth and planar, as observed with scanning electron microscopy (SEM), indicating a layer-by-layer growth typical of transition metal dichalogenides.