Surface Insights of Mesoporous Fragile Organic Materials Under Ultra‐Low‐Voltage Directed by Gemini Column

Abstract Mesoporous materials find widespread applications due to their high specific surface area, contributing to enhanced performance. Scanning electron microscopy (SEM) observation of mesoporous materials provides valuable insights into their mesostructures. However, direct observation of the outermost surfaces, which often dictate material properties, remains challenging, especially for highly insulating and fragile compounds. In this study, utilizing SEM observation with ultra‐low‐voltage acceleration directed by Gemini column is proposed to achieve direct surface imaging of mesoporous organic materials with highly insulating and fragile characteristics. By observing mesostructured polymers obtained through a soft‐templating method without washing, stuffed pores are identified allowing the differentiation of micelle templates and polymer walls. Moreover, leveraging SEM measurements, a polymerization mechanism is proposed for dopamine on the polymer micelles adhered to the graphene oxide nanosheets. These findings demonstrate the potential of SEM measurements with ultra‐low accelerating voltage in facilitating surface observations of polymer‐derived nanomaterials characterized by high insulating properties and a fragile framework.