Abstract: Graphdiyne was prepared by a cross coupling reaction and characterized by SEM, TEM, XRD, Raman spectroscopy and XPS. Its photoluminescence (PL) properties were investigated. It was found that the graphdiyne has a thickness of ca. 1 μm, a O/C atomic ratio of ca. 0.174 1 and many oxygen-containing functional groups. It exhibits strong ultraviolet (UV) PL at 397 nm and optical absorption at ca. 280 nm. It is proposed that the oxygen-containing functional groups in the graphdiyne induce charge transfer, leading to the PL properties. As a new kind of artificially synthesized carbon allotrope, graphdiyne with UV PL have many applications.