Electrodeposition of MoS₂ from dichloromethane

Abstract

The electrodeposition of MoS₂ from dichloromethane (CH₂Cl₂) using tetrabutylammonium tetrathiomolybdate ([NⁿBu₄]₂[MoS₄]) as a single source precursor is presented. The electrodeposition of MoS₂ from CH₂Cl₂ requires addition of a proton donor to the electrolyte and trimethylammonium chloride (Me₃NHCl) 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 MoS₂ and anodic deposition of MoS₃ as well as an additional corrosion process where the deposited MoS₃ strips back into solution. The electrodeposited MoS₂ 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 MoS₂ 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.

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Identifiers

ORCID for Shibin Thomas: orcid.org/0000-0002-7735-788X

ORCID for Danielle E. Smith: orcid.org/0000-0002-2446-1763

ORCID for Victoria Greenacre: orcid.org/0000-0002-3381-9616

ORCID for Yasir Noori: orcid.org/0000-0001-5285-8779

ORCID for Andrew L. Hector: orcid.org/0000-0002-9964-2163

ORCID for Cornelis De Groot: orcid.org/0000-0002-3850-7101

ORCID for Gillian Reid: orcid.org/0000-0001-5349-3468

ORCID for Philip N. Bartlett: orcid.org/0000-0002-7300-6900

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