The acetylenic carbon-rich nanostructures such as graphdiyne has been received increasing attentions due to its potential applications in energy conversion, photoelectronic devices, catalysis, sensing and biomedical areas. So, development of facile synthesis procedures for ultrathin graphdiyne nanostructures is a challenge. Here, a prompt and simple method is proposed for polycondensation of 1,3,5-triethynylbenezene and synthesis of graphdiyne-like nanosheets, using bipolar electrochemistry assisted by copper grid electrode in the ethanol/acetonitrile solvent. The large scale of graphdiyne can be achieved with a series of bipolar electrodes in a single bipolar cell. The prepared nanosheets are characterized by various techniques, such as SEM, TEM, Raman and XPS. The as prepared material shows a remarkable photocatalytic activity toward hydrogen evolution (25 mA cm2 at 0.6 V vs. RHE) as well as oxygen evolution (4.5 mA cm2 at 1.1 V vs. RHE) activity at low overpotentials. The proposed method promised as a rapid and simple process for synthesis of graphdiyne-like nanostructures with remarkable electrocatalytic activity at less than 150 min. Furthermore, the presented procedure can be developed as applicable method for preparation of other grphdiyne-like nanostructures for fabrication of sensing and biosensing devices, optical imaging and nanoparticles loading.
