Micro-electromechanical system-based cryogenic and heating in situ transmission electron microscopy for investigating phase transitions and domain evolution in single-crystal BaTiO3

Investigating phase transitions between ferroelectric states is crucial for understanding the nucleation, dynamics, and kinetics of domains, both before and after transformation. Here, we assess all phase transitions and domain evolutions in single-crystal BaTiO3 by implementing microelectromechanical systems (MEMS)-based in situ cryogenic (cryo-) and heating transmission electron microscopy (TEM) by continuously varying sample temperatures from -175 °C to 200 °C. Every possible phase-cubic, tetragonal, orthorhombic, and rhombohedral - was identified. An ultra-stable imaging condition was achieved with a mean drift speed of 1.52 nm/min, providing unique opportunities for atomic resolution in situ scanning TEM with a wide temperature range. Furthermore, domain nucleation and evolution across phase transitions were investigated using complementary dielectric measurements, optical microscopy, and a phenomenological model. This study underscores the effectiveness and utility of MEMS-based in situ cryo-/heating TEM in revealing phase transitions and domain structures in ferroelectric materials.