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Ultrafast synchrotron X-ray imaging and multiphysics modelling of liquid phase fatigue exfoliation of graphite under ultrasound

Qin, Ling; Maciejewska, Barbara M.; Subroto, Tungky; Morton, Justin A.; Porfyrakis, Kyriakos; Tzanakis, Iakovos; Eskin, Dmitry G.; Grobert, Nicole; Fezzaa, Kamel; Mi, Jiawei


Ling Qin

Barbara M. Maciejewska

Tungky Subroto

Justin A. Morton

Kyriakos Porfyrakis

Iakovos Tzanakis

Dmitry G. Eskin

Nicole Grobert

Kamel Fezzaa


Ultrasound-assisted liquid phase exfoliation is a promising method for manufacturing of 2D materials in large scale and sustainable manner. A large number of studies using ex-situ nano/micro structural characterization techniques have been made to investigate the underlying mechanisms, aiming to understand the exfoliation dynamics. Due to the complex multiphysics and multi-length nature of the process, those ex-situ methods cannot provide the real-time and in-situ dynamic information for understanding how exactly layer exfoliation starts and grows under ultrasound. Here, we used the ultrafast synchrotron-X-ray phase-contrast imaging (a combined temporal resolution of 3.68 μs and a spatial resolution of 1.9 μm/pixel) to study the exfoliation dynamics in real time and operando condition. We revealed, for the first time, the fatigue exfoliation phenomenon at the graphite surface caused by the imploding ultrasonic bubbles occurring cyclically in line with the ultrasound frequency. A multiphysics numerical model was also developed to calculate the shock wave produced at bubble implosion and the resulting cyclic and impulsive tensile and shear stresses acting on the graphite surface. Our research reveals that the graphite layer exfoliation rate and efficiency are predominantly determined by the number of imploding bubbles inside the effective cavitation bubble zone. The findings are valuable for developing industrial upscaling strategies for ultrasound processing of 2D materials.


Qin, L., Maciejewska, B. M., Subroto, T., Morton, J. A., Porfyrakis, K., Tzanakis, I., …Mi, J. (2022). Ultrafast synchrotron X-ray imaging and multiphysics modelling of liquid phase fatigue exfoliation of graphite under ultrasound. Carbon, 186, 227-237.

Journal Article Type Article
Acceptance Date Oct 4, 2021
Online Publication Date Oct 7, 2021
Publication Date 2022-01
Deposit Date Jan 14, 2022
Publicly Available Date Jan 14, 2022
Journal Carbon
Print ISSN 0008-6223
Publisher Elsevier
Peer Reviewed Peer Reviewed
Volume 186
Pages 227-237
Keywords Ultrafast synchrotron X-ray phase-contrast imaging; 2D layered graphite materials; multi-physics modelling; liquid-phase exfoliation; ultrasound exfoliation dynamics
Public URL
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Copyright Statement
© 2021 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY licence

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