A Deprotection‐free Method for High‐yield Synthesis of Graphdiyne Powder with In Situ Formed CuO Nanoparticles

With a direct band gap, superior charge carrier mobility, and uniformly distributed pores, graphdiyne (GDY) has stimulated tremendous interest from the scientific community. However, its broad application is greatly limited by the complicated multistep synthesis process including complex deprotection of hexakis‐[(trimethylsilyl)ethynyl]benzene (HEB‐TMS) and peeling of GDY from the substrates. Here, we describe a deprotection‐free strategy to prepare GDY powder by directly using HEB‐TMS as the monomer. When CuCl was used as the catalysts in DMF solvent, the yield of GDY powder reached ≈100 %. More interestingly, uniformly dispersed CuO nanoparticles with an average diameter of ≈2.9 nm were in situ formed on GDY after the reaction. The prepared CuO/GDY was demonstrated an excellent co‐catalyst for photocatalytic hydrogen evolution, comparable to the state‐of‐art Pt co‐catalyst. The deprotection‐free approach will widen the use of GDY and facilitate its scaling up to industrial level.