MoS₂, a key material for supercapacitors, batteries, photovoltaics, catalysis, and sensing applications, was synthesized using the hydrothermal method. Different precursors such as molybdenum sources (ammonium heptamolybdate tetrahydrate ((NH₄)₆Mo₇O₂₄·4H₂O) and sodium molybdate hydrate (Na₂MoO₄·2H₂O)) combined with L-cysteine, thiourea, and thioacetamide, as the sulfur source, were involved. The obtained samples were morphologically and structurally characterized by X-ray diffraction, Raman spectroscopy, N₂ adsorption/desorption measurements, and Scanning Electron Microscopy with Energy-Dispersive X-ray Spectroscopy (SEM–EDX). Electrochemical impedance spectroscopy was involved in MoS₂ characterization as electrode materials. The objective of this study was to ascertain the impact of precursor combinations on the morphological, structural, and electrochemical characteristics of MoS₂. A thorough examination of the empirical data revealed that the MoS₂ compounds, which were synthesized using thiourea as the sulfur source, exhibited a more pronounced flower-like morphology, increased crystallite size, and enhanced electrochemical properties with potential electrochemical applications.

Advances in energy storage and energy conversion play an essential role nowadays because the energy demands are becoming greater than ever. To overcome the actual performances of the materials used to build supercapacitors, a combination of transition metal dichalcogenides (TMDCs) and graphene oxide (GO) or reduced graphene oxide (rGO) as graphene-based structures are often studied for their excellent properties, such as high specific area and good electrical conductivity. Nevertheless, synthesis pathways and parameters play key roles in obtaining better materials as components for supercapacitors with higher technical performances. Driven by the desire to understand the influence of the structural and morphological particularities on the performances of supercapacitors based on MoS₂/graphene oxide (GO) composites, a survey of the literature was performed by pointing out the alterations induced by different synthesis pathways and key parameters to the above-mentioned particularities.