| Summary: | Sulfur-doped carbon nanohorns (S-CNHs) were prepared by an easy one-pot solvothermal process and were employed as efficient electrocatalysts towards water splitting. Initially, oxidation of CNHs followed by thermal treatment with the Lawesson’s reagent resulted in the formation of S-CNHs with the sulfur content determined as high as 3%. The S-CNHs were thoroughly characterized by spectroscopic, thermal and electron microscopy imaging means and then electrocatalytically screened. Specifically, S-CNHs showed excellent activity and durability for both O<sub>2</sub> and H<sub>2</sub> evolution reactions, by showing low overpotential at 1.63 and −0.2 V vs. RHE for oxygen and hydrogen evolution reaction, respectively. Additionally, S-CNHs showed significantly lower Tafel slope value and lower current resistance compared to oxidized and pristine CNHs for both electrocatalytic reactions. The outstanding electrocatalytic properties and high conductivity, along with the high S-doping level, render S-CNHs a promising bifunctional electrocatalyst for water splitting.
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