Extending the operating window of scanning electron microscopy through an integrated electron-optical architecture for high-temperature and near-ambient-pressure environments

Abstract

Scanning electron microscopy (SEM) under simultaneously high-temperature, near-ambient-pressure (NAP), and reactive-gas environments requires coordinated control of vacuum isolation, electron-beam transmission, signal generation, and thermal management, constraints that have long limited the operating window of environmental scanning electron microscopy (ESEM). Here we establish an integrated electron-optical architecture that combines a multistage differential-pressure pathway, front-stage pressure transition, detector optimization, thermal management, and a gas-focusing sampling architecture into a unified ESEM platform. Pressure distribution and electron-beam transmission are quantitatively validated through computational fluid dynamics (CFD), Monte Carlo electron-gas scattering analysis, and direct beam-current measurements, while detector optimization and thermionic-electron suppression preserve stable imaging under elevated pressure and temperature. The resulting system enables stable SEM imaging at pressures up to 20,000 Pa and high-temperature imaging up to 1,400 degrees C, continuous observation of hydrated biological specimens, and synchronized SEM-QMS operando characterization using local gas sampling. These developments establish a general electron-optical framework for extending ESEM toward realistic operando environments where elevated temperature, reactive gases, structural evolution, and gas-phase chemistry can be investigated simultaneously.