Ultrasound cavitation and exfoliation dynamics of 2D materials re-vealed in operando by X-ray free electron laser megahertz imaging

Ultrasonic liquid phase exfoliation is a promising method for the production of 2D layered materials. A large number of studies have been made in investigating the underlying ultrasound exfoliation mechanisms. Due to the experimental challenge in capturing in real-time the highly transient and dynamic phenomena in sub-microsecond time scale and micrometer length scale at the same time, most theories reported to date are still under intensive debate. Here, we report the exciting new findings from the first scheduled user experiment using the free electron laser MHz X-ray Microscopy at the SPB/SFX instrument of the European X-ray Free-Electron Laser. The ultra-short X-ray pulse (~25 fs) and the unique pulse train time structure allow us to reveal fully the ultrasound cavitation dynamics, including the nucleation, growth, implosion dynamics of cavitation bubbles at different wave amplitudes. Using ma-chine-learning image processing, the instance of bubble cloud shock wave emission, their periodic impact onto the graphite materials and the cyclic fatigue exfoliation mechanism in multi-time scale from sub-microsecond to tens of minutes were all quantified and elucidated in this research.