On the basis of the design and synthesis of functional molecules, considering the key scientific issues of energy principle, match between structure and properties, and complex physical and chemical phenomena at small-scale, the new self-assembly methods were established to develop self-assembly techniques for molecular aggregation materials with controllable sizes and structures, and some large area, highly ordered molecular aggregation materials were constructed. Ordered heterogeneous and homogeneous materials and surface/interface issues, especially interface activity, interface connecting were investigated. The strong dependence of property and functionality on the morphology, size and dimension in the molecular aggregation materials was proved. The synthesis method for a new allotrope of carbon, graphydiyne, was established, the first successful synthesis of two-dimensional carbon allotrope graphydiyne with band gap of 0.46 eV on the copper foil was achieved, and the application of graphydiyne in the area of information technology, electronics, energy, catalysis and photovoltaic were investigated. These studies are of great scientific significance on chemistry, materials science, physics, microelectronics and other basic scientific research and related interdisciplinary areas, showing important academic value and potential applications in the area of micro-nano electronics, field emission, photoelectric conversion and biosensors.