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Chemomechanical interactions in gas or liquid environments are crucial forthe functionality and longevity of various materials used in sustainable energytechnologies, such as rechargeable batteries, water-splitting catalysts, andnext-generation nuclear reactors. A comprehensive understanding of nanoscalestrain evolution involved in these processes can advance our knowledge ofunderlying mechanisms and facilitate material design improvements. However,traditional microscopy workflows face challenges due to trade-offs betweenfield of view (FOV), spatial resolution, temporal resolution, and electron beamdamage, particularly in gas or liquid environments. Here, we demonstrate insitu nanometer-resolution strain and orientation mapping in atemperature-controlled gas environment with a large FOV. This is achieved byintegrating a microelectromechanical system (MEMS)-based closed-cell TEMholder, precession-assisted four-dimensional scanning transmission electronmicroscopy (4D-STEM), and a direct electron detector (DED). Using the strainevolution during zirconium initial oxidation as a case study, we first outlinecritical strategies for focused ion beam gas-cell sample preparation andgas-phase TEM workflows to enhance experimental success. We then show thatintegrating DED with precession electron diffraction and optimizing gaspressure substantially improve the quantity and quality of the detected Braggpeaks in nano-beam electron diffraction patterns, enabling more precise strainmeasurements. Furthermore, we introduce a practical protocol to pause thereactions, allowing sufficient time for 4D-STEM data collection while ensuringthe temporal resolution needed to resolve material dynamics. Our methodologyand workflow provide a robust framework for quantitative analysis ofchemomechanical evolutions in materials exposed to gas or liquid environments.

In Situ Nanometer-Resolution Strain and Orientation Mapping for  Gas-Solid Reactions via Precession-Assisted Four-dimensional Scanning  Transmission Electron Microscopy