Abstract: | Graphyne (GY) is a new type of carbon allotrope, which is viewed as a rapidly rising star in the carbon family referred to as 2D carbon allotropes due to its extraordinary properties. Considering the dynamic nature of the alkyne metathesis reaction, a hydrogen‐substituted graphyne (HsGY) film is successfully synthesized on a gas/liquid interface using 1,3,5‐tripynylbenzene (TPB) as the precursor. The synthesized HsGY film is used as a sulfur host matrix to be applied in lithium–sulfur batteries (LSBs). The HsGY@S electrode is prepared using S8 as sulfur source and presents excellent electrochemical performance. |