摘要： Synthesis of free standing two-dimensional (2D) conjugated covalent organic framework (COF) films linked by C-C bonds can be considered as a holy grail of synthetic chemistry. However, reactions for their synthesis are quite rare. Herein we developed a very simple and mild strategy to synthesize them via the Nobel Prize reaction (Suzuki polymerization) on water/toluene interface in a fridge. The versatility of this strategy was proved by the successful synthesis of two different 2D-COF films: a porous graphene and a porphyrin-contained 2D-COF. Both 2D-COF films have large lateral size and their crystalline domains were visualized by high resolution TEM. Based on the wide compatibility of Suzuki reaction, our breakthrough work opened a door for the synthesis of various 2D conjugated COF films. For application studies, the porous graphene exhibits a good carrier mobility which is much higher than -C=N- linked 2D COF films and a good catalytic activity for hydrogen evolution reaction which is comparable with nitrogen or phosphorus doped graphene.