Colloidal synthesis of rhenium disulfide nanosheets enables a simple and cost‐effective exploitation of its peculiar layer‐independent properties for gas‐sensing and electrochemical H2 production. The surface functionalization of the nanosheets leads to sensitive and fast response gas sensors, while their assembly with carbon nanotubes enhances its electrocatalytic activity, making both device performances competitive with chemical vapor deposition rhenium disulfide. Abstract Among the large family of transition metal dichalcogenides, recently ReS2 has stood out due to its nearly layer‐independent optoelectronic and physicochemical properties related to its 1T distorted octahedral structure. This structure leads to strong in‐plane anisotropy, and the presence of active sites at its surface makes ReS2 interesting for gas sensing and catalysts applications. However, current fabrication methods use chemical or physical vapor deposition (CVD or PVD) processes that are costly, time‐consuming and complex, therefore limiting its large‐scale production and exploitation. To address this issue, a colloidal synthesis approach is developed, which allows the production of ReS2 at temperatures below 360 °C and with reaction times shorter than 2h. By combining the solution‐based synthesis with surface functionalization strategies, the feasibility of colloidal ReS2 nanosheet films for sensing different gases is demonstrated with highly competitive performance in comparison with devices built with CVD‐grown ReS2 and MoS2. In addition, the integration of the ReS2 nanosheet films in assemblies together with carbon nanotubes allows to fabricate electrodes for electrocatalysis for H2 production in both acid and alkaline conditions. Results from proof‐of‐principle devices show an electrocatalytic overpotential competitive with devices based on ReS2 produced by CVD, and even with MoS2, WS2, and MoSe2 electrocatalysts.

Published in: "Small".