Cs-corrected cryo-TEM with inert-gas protection for atomic characterization of dual air- and beam-sensitive materials

Cryogenic transmission electron microscopy (cryo-TEM) has revolutionized life sciences, yet its application in materials research remains limited, leaving much of its potential untapped. This gap arises from a lack of awareness of cryo-TEM’s unique capabilities beyond biology and the absence of reliable workflows tailored to electron-beam-sensitive materials. Here, we develop a Cs-corrected cryo-TEM platform integrated with an inert-gas glovebox integrated system (GIS), enabling seamless, air-free transfer of air-sensitive samples from an inert atmosphere to the cryogenic vacuum environment. We established a complete methodology for low-dose, atomic-resolution imaging and post-processing of dose-fractionated subframe stacks. Using emerging whereas extremely air-sensitive (4-fluorobenzylamine (FB)) 2 MnCl 4 , organic–inorganic hybrid perovskites and NbOI 3 1D ferroelectric crystals as model systems, we demonstrate the capability of this approach to resolve structural and chemical features previously inaccessible due to dual air and beam sensitivity. Our workflow provides a generalizable and reproducible pathway for high-resolution imaging and elemental analysis of fragile novel materials, offering a powerful tool to accelerate the discovery and structure–property understanding of next-generation functional materials.