The practical applications of lithium–sulfur batteries are still a great challenge due to the polysulfide shuttle and capacity decay. Herein, we report a NiO–carbon nanotube/sulfur (NiO–CNT/S) composite by hydrothermal and thermal treatments. This hybrid combines the high conductivity of CNTs and double adsorption of CNTs and NiO (physical and chemical adsorption) to improve the electrochemical performance for the sulfur electrodes. Compared with CNT/S and NiO/S, the developed NiO–CNT/S composites present a preferable initial reversible discharge capacity (1072 mA h g⁻¹) and is maintained at 609 mA h g⁻¹ after 160 cycles at 0.1C.