Abstract: The mechanism of intermolecular electronic cloud sharing determines the strength of intermolecular interaction (chemical bond formation). According to this mechanism, a new instrumental device for regulating the nanoscale molecular assembly process was designed and developed. Visual monitoring methods such as laser particle size analysis and high-speed imaging systems are innovatively integrated into the instrument, realize real-time online monitoring of the electrodelation reaction, product formation process and recording the characteristics of the desolvation process. Study the effects of essential properties of molecules (such as molecular structure, polarity, volatility, electron-negativity), coexisting substrates (such as solvents, other coexisting materials), and environmental parameters (such as temperature, pressure, distance, electric field) on the assembly process of different particles (such as neutral molecules, positive ions, negative ions), and energy-related dynamics. At present, the rapid controllable crystallization of ultra-dilute NaCl solution, the morphology and size adjustment of nano-gold, the preparation of nanowire arrays such as Pd/TiO₂ and the films of ZnFe₂O₄, and so on, have been achieved. It has shown good development prospects in the structural synthesis and preparation of inorganic functional materials.