This work investigates the possibility and potential insights gained from in-situ scanning electron microscopy (SEM) experiments focused on the dynamic heating of CaCO3 for calcination processes. MEMS chips were used to facilitate uniform heating, precise control of heating parameters and reproducibility, providing a controlled environment for comprehensive experimentation. This work focuses on the microstructure transformation, with particular emphasis on the meso- and macropores, grain formation, and the sintering behavior of these particles. Influence of heating rates and complex interplay of temperature and microstructural transformations was revealed. The results obtained may be useful for optimization and microstructural-based design of the calcination procedures for complex process engineering in various applications.