Abstract: The invention discloses a method for the synthesis of monodispersed luminescent quantum dots of transition metal dichalcogenides (TMDC), single- or few-layered, using a single-step electrochemical exfoliation that involves dilute ionic liquid and water. The method disclosed helps to obtain nanoclusters of TMDC of desired size including small sizes ranging up to 6 nm, by varying the concentration of the electrolyte and the applied DC voltage. The invention further discloses a method by which mono- or few-layered luminescent transition metal dichalcogenides can be directly deposited onto conducting substrates in a uniform manner. The monodispersed single- or few-layered luminescent TMDC and electro-deposited substrates exhibit improved electronic conductivity and new active sites, making them suitable as high-performance electrocatalysts in hydrogen evolution reactions in solar water-splitting applications and also as electrodes for solar cell applications.