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Graphdiyne (g−CnH2n‐2), a novel two‐dimension carbon allotrope material composed of a sp‐ and sp2‐hybrid carbon network, has been widely explored since it was synthesized for the first time by Li's group in 2010. A series distinct and excellent properties bestow graphdiyne excellent performance in many fields. Here, an innovative progress for preparing graphdiyne by using Cu+ contained material as catalyst is reported and the composite CuI‐GD is coupled with flower‐like NiAl‐LDH to produce H2 from photocatalytic water splitting. The results of FTIR and Raman spectroscopy together reveal that graphdiyne nanosheets are synthesized successfully by employing a cross‐coupling method. Photocatalytic hydrogen evolution performance shows that the hydrogen production activity of CuI‐GD/NiAl‐LDH has a 15‐ and 216‐fold enhancement compared with CuI‐GD and NiAl‐LDH, respectively. A series of characterizations are carried out to expound the underlying reasons in the enhancement of the photocatalytic hydrogen production performance of CuI‐GD/NiAl‐LDH. Meanwhile, a possible mechanism for the photocatalytic hydrogen evolution process was proposed to understand the interaction among these materials. [ABSTRACT FROM AUTHOR]