Vacuum‐Nitrogen Assisted (VANS) Topotactical Deintercalation for Extremely Fast Production of Functionalized Silicene Nanosheets

Abstract Silicene, the analog of graphene composed of silicon atoms arranged in a honeycomb lattice, has garnered significant attention due to its unique properties, positioning it as a promising candidate for various applications in electronic devices, photovoltaics, photocatalysis, and biomedicals. While the chemical synthesis of silicene nanosheets has traditionally involved time‐spending and expensive‐ methods, this study introduces a rapid vacuum/nitrogen cycle assisted (VANS) protocol that dramatically speeds up the production of silicene. The strategic implementation of vacuum/nitrogen cycles provides the efficient removal of the generated hydrogen, boosting the overall reaction kinetics while maintaining inert reaction conditions to prevent oxidation. In contrast to previous methodologies, usually qualified by prolonged reaction durations of up to 5 days and low reaction temperatures (−30 °C), this integrated approach substantially shortens the synthesis time from hours to minutes. Indeed, the VANS method drastically reduces the reaction time, operates at room temperature, and exhibits the successful fabrication of silicene flakes with structural properties comparable to those achieved through prolonged reaction times and low temperatures.