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Ultrasound-assisted liquid-phase exfoliation is a promising method for manufacturing two-dimensional materials. Understanding the effect of ultrasonication parameters such as the temperature and input power on the developed pressure field is pivotal for optimization of the process. Limited research has been carried out to determine the optimal temperature for exfoliation, with some data generating disputed results. Simply maximizing the sonication power does not necessarily produce a higher yield because of shielding. In this study, a high-temperature calibrated cavitometer was used to measure the acoustic pressure generated in different graphite solutions in deionized water at various temperatures (from 10°C to 70°C) and input power conditions (from 20% to 100%). In addition, high-speed optical imaging provided insight on the shock wave generation from transient bubble collapses under different sonication conditions. The optimal sono-exfoliation parameters were determined to be 20% input power at 10°C for graphite flake solution, and 100% input power at 40°C to 50°C for graphite powder solution.

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Ultrasonic cavitation is used in various processes and applications, utilising powerful shock waves and high-speed liquid jets generated by the collapsing bubbles. Typically, a single frequency source is used to produce the desired effects. However, optimisation of the efficiency of ultrasound reactors is necessary to improve cavitation activity in specific applications such as for the exfoliation of two dimensional (2D) materials. This research takes the next step to investigate the effect of a dual frequency transducer system on the bubble dynamics, cavitation zone, pressure fields, acoustic spectra and induced shock waves for four liquids with a range of physical properties. Using ultra-high-speed imaging and synchronised acoustic pressure measurements, the effect of ultrasonic dual frequencies on bubble dynamics was investigated. The addition of a high frequency transducer (1174 kHz) showed that the bubble fragments and satellite bubbles induced from a low frequency transducer (24 kHz) were able to extend their lifecycle, increase spatial distribution, thus, extending the boundaries of the cavitation zone. Furthermore, this combination of ultrasonic frequencies generated higher acoustic pressures (up to 180%) and enhanced the characteristic shock wave peak, indicating more bubble collapses and the generation of additional shock waves. The dual frequency system also enlarged the cavitation cloud size under the sonotrode. These observations specifically delineated the enhancement of cavitation activity using a dual frequency system pivotal for optimisation of existing cavitation-based processing technologies.