Professor Iakovos Tzanakis

Ultrasonic cavitation processing (USP) is a versatile technique that has gained a lot of momentum in the last decade as a sustainable, environmentally friendly, and cost-effective process. USP uses high-frequency sound to form bubbles that expand, contract, and eventually collapse, generating high-speed liquid jets, powerful shockwaves, and acoustic streaming effects. Despite its widespread application, use of USP remains mostly empirical. For processes involving the synthesis and production of materials, harnessing the power of cavitation requires an understanding of the fundamental mechanisms driving USP. In this presentation, we record recent studies to analyse, optimise, and control USP for applications related to grain refinement of aluminium alloys, exfoliation of 2D nanomaterials, and processing of composites. High-speed cameras and in situ synchrotron imaging were used to visualise cavitation dynamics, coupled with state-of-the-art hydrophones to detect acoustic waves and shockwave emissions. Results show that optimised USP with the help of advanced modelling significantly improves grain refinement of aluminium alloys in processes such as direct-chill (DC) casting, where shockwaves are primarily responsible for the fragmentation of intermetallic crystals/dendrites. Furthermore, shockwaves act as the main driving mechanism for the exfoliation of 2Ds while cavitation activity enhances fibre dispersion in highly viscous polymers, improving matrix stability and strength.

This paper follows our earlier work where a strong high frequency pressure peak has been observed as a consequence of the formation of shock waves due to the collapse of cavitation bubbles in water, excited by an ultrasonic source at 24 kHz. We study here the effects of liquid physical properties on the shock wave characteristics by replacing water as the medium successively with ethanol, glycerol and finally a 1:1 ethanol–water solution. The pressure frequency spectra obtained in our experiments (from more than 1.5 million cavitation collapsing events) show that the expected prominent shockwave pressure peak was barely detected for ethanol and glycerol, particularly at low input powers, but was consistently observed for the 1:1 ethanol–water solution as well as in water, with a slight shift in peak frequency for the solution. We also report two distinct features of shock waves in raising the frequency peak at MHz (inherent) and contributing to the raising of sub-harmonics (periodic). Empirically constructed acoustic pressure maps revealed significantly higher overall pressure amplitudes for the ethanol–water solution than for other liquids. Furthermore, a qualitative analysis revealed that mist-like patterns are developed in ethanol–water solution leading to higher pressures.

Ultrasonic cavitation is used in various processes and applications, utilizing 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, optimization of the efficiency of ultrasound reactors is necessary to improve cavitation activity in specific applications such as for the exfoliation of two dimensional 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 synchronized 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 and 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 optimization of existing cavitation-based processing technologies.

This work deals with the measurement of mechanical properties of single and polycrystalline Al3Zr specimens from ambient to elevated temperatures using nano-indentation experiments. In this study, we employed three kinds of intermetallic specimens produced from Al3Zr crystals chemically extracted from an Al-3 wt% Zr alloy. The properties such as elastic modulus and hardness were determined under quasistatic loading conditions. Constant multicycle indentation testing (MCT) was further performed using a Vickers indenter to understand the fatigue response of intermetallics at high load low cycle conditions. The results showed that hardness and elastic modulus of Al3Zr intermetallics depended on the crystal structure/orientation, with polycrystalline samples showing higher elastic modulus than single crystal specimens at room temperature conditions. MCT experiments revealed that contact pressure of more than 7 GPa was needed to fracture a crack-free crystal under dynamic loading conditions. Consequently the properties of intermetallics at temperatures up to 700 °C were determined for the first time, using high-temperature nano-indentation technique. Elevated temperature measurements indicated that intermetallics had high creep resistance at low and intermediate temperatures, but exhibited significant plastic deformation and creep close to the melting point of pure aluminium.

Ultrasonic assisted liquid phase exfoliation (ULPE) is a promising method for the large scale production of 2D materials. Currently, toxic solvents such as N-Methyl-2-pyrrolidone (NMP) are commonly used for the production of graphene. In this paper four solvents; three green solvents (water, ethanol and water/ethanol) plus NMP for comparison, were sonicated and examined in terms of their bubble dynamics and acoustic emissions. Advanced fundamental analysis was conducted using high-speed imaging synchronised with acoustic pressure measurements complemented by shadowgraphic photography of the emitted shockwaves, in order to determine a suitable eco-friendly solvent medium from a cavitation bubbles dynamics perspective. Thereafter, ULPE of graphite in the optimum solvent took place for 2 h under controlled ultrasonication parameters. The produced graphene samples were characterised by employing a series of techniques consisting of Ultraviolet–visible (UV–Vis) and Raman spectroscopy as well as transmission electron microscopy (TEM). A mixture of deionised water and ethanol was shown to produce a yield twice that of pure water, comprising of high quality few layer graphene (3–5 Ls) with an average area of ∼1.15 (μm)2 and stability of ∼78% for the duration of six months. This combination is a promising eco-friendly substitute for future commercial manufacturing of graphene.

Ultrasonic melt processing (USP) has been known for decades for beneficial effects in as-cast aluminium alloys, including degassing, grain and structure refinement. In the last 10 years the authors performed a series of research projects dedicated to understanding the nature of these effects, by dedicated advanced experiments and by developing numerical models that adequately reflect the complicated physics involved, aiming at further optimising the technology so that it becomes feasible for scale-up applications and attractive for industrial use. Based on the main USP mechanisms previously studied by in-situ observations coupled with acoustic pressure measurements, i.e. fragmentation, deagglomeration and dispersion of the solid phases and inclusions, technological approaches are suggested and tested for grain refinement upon direct-chill casting of Al alloys. Results showed that USP in the melt flow in the launder significantly improves the as-cast structure of a billet, opening the way for upscaling.

Graphene dispersions in water are highly desirable for a range of applications such as biomedicines, separation membranes, coatings, inkjet printing and more. Recent novel research has been focussed on developing a green approach for scalable production of graphene. However, one important parameter, which is often neglected is the bulk temperature of the processing liquid. This paper follows our earlier work where optimal sono-exfoliation parameters of graphite in aqueous solutions were determined based on the measured acoustic pressure fields at various temperatures and input powers. Here, we take the next step forward and demonstrate using systematic characterisation techniques and acoustic pressure measurements that sonication-assisted liquid phase exfoliation (LPE) of graphite powder can indeed produce high quality few layer graphene flakes in pure water at a specific temperature, i.e. 40 °C, and at an optimised input generator power of 50%, within 2-h of processing. UV–vis analysis also revealed that the exfoliation, stability and uniformity of dispersions were improved with increasing temperature. We further confirmed the successful exfoliation of graphene sheets with minimal level of defects in the optimized sample with the help of Raman microscopy and transmission electron microscopy. This study demonstrated that understanding and controlling processing temperature is one of the key parameters for graphene exfoliation in water which offers a potential pathway for its large-scale production.

The impregnation of continuous carbon fibre roving with thermoplastic melt is a challenging task due to the high viscosity and surface tension of the melt. A new technique is under development utilizing ultrasonic oscillations within the thermoplastic melt which encloses a fibre roving, to achieve fibre impregnation. Despite ultrasonic processing being very efficient, the specific conditions created in the thermoplastic melt have never been studied before. This study investigated whether cavitation effects could be present during ultrasound-assisted fibre impregnation. The observed acoustic effects allowed us to suggest the possible underlying mechanisms. For the purpose of the study a melt-bath impregnation setup with polylactide was built. To detect the cavitation effects and acoustic parameters a calibrated high-temperature cavitometer was used. The results showed the formation of small cavitation zones in the direct vicinity to the sonotrode tip where the fibre roving would be positioned. Therefore, the occurrence of cavitation was established, and induced effects like shock waves, microjets and microstreaming should be further considered for detailed investigation of the ultrasound-assisted impregnation mechanism.

Grain refinement in alloys is a well-known effect of ultrasonic melt processing. Fragmentation of primary crystals by cavitation-induced action in liquid metals is considered as one of the main driving mechanisms for producing finer and equiaxed grain structures. However, in-situ observations of the fragmentation process are generally complex and difficult to follow in opaque liquid metals, especially for the free-floating crystals. In the present study, we develop a transparent test rig to observe in real time the fragmentation potential of free-floating primary Al3Zr particles under ultrasonic excitation in water (an established analogue medium to liquid aluminium for cavitation studies). An effective treatment domain was identified and fragmentation time determined using acoustic pressure field mapping. For the first time, real-time high-speed imaging captured the dynamic interaction of shock waves from the collapsing bubbles with floating intermetallic particles that led to their fragmentation. The breakage sequence as well as the cavitation erosion pattern were studied by means of post-treatment microscopic characterisation of the fragments. Fragment size distribution and crack patterns on the fractured surface were then analysed and quantified. Application of ultrasound is shown to rapidly (

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.

Ultrasonic de-agglomeration and dispersion of oxides is important for a range of applications. In particular, in liquid metal, this is one of the ways to produce metal-matrix composites reinforced with micron and nano sized particles. The associated mechanism through which the de-agglomeration occurs has, however, only been conceptualized theoretically and not yet been validated with experimental observations. In this paper, the influence of ultrasonic cavitation on SiO2 and MgO agglomerates (commonly found in lightweight alloys as reinforcements) with individual particle sizes ranging between 0.5 and 10 μm was observed for the first time in-situ using high-speed imaging. Owing to the opacity of liquid metals, a de-agglomeration imaging experiment was carried out in de-ionised water with sequences captured at frame rates up to 50 kfps. In-situ observations were further accompanied by synchronised acoustic measurements using an advanced calibrated cavitometer, to reveal the effect of pressure amplitude arising from oscillating microbubbles on oxide de-agglomeration. Results showed that ultrasound-induced microbubble clusters pulsating chaotically, were predominantly responsible for the breakage and dispersion of oxide agglomerates. Such oscillating cavitation clusters were seen to capture the floating agglomerates resulting in their immediate disintegration. De-agglomeration of oxides occurred from both the surface and within the bulk of the aggregate. Microbubble clusters oscillating with associated emission frequencies at the subharmonic, 1st harmonic and low order ultra-harmonics of the driving frequency were deemed responsible for the breakage of the agglomerates.

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.

Ultrasound-aided liquid phase exfoliation (ULPE) of graphene in pure water is environment-friendly. Two limiting factors of ULPE are the non-uniform thickness of few-layer graphene (FLG) and a relatively low graphene yield. Here we describe ULPE in water that enables us to produce FLG flakes with a thickness of 3 layers and the flake sizes exceeding 1 μm2 in just 2 h. This process is based on using a combination of two ultrasound sources of high and low frequencies: 1174 kHz and 20 kHz. Two different frequencies generate a wider population and size distribution of cavitation bubbles that act through a number of mechanisms towards the exfoliation of graphene. For the first time ULPE was characterized by acoustic measurements. Results show that a high graphene yield (10%) can be achieved. This study demonstrates that the use of a dual frequency ultrasonic source and control of acoustic pressure is critical in optimizing the quality and yield of the cavitation assisted LPE of graphene in pure water. It is suggested that the width of the acoustic pressure peak reflecting shock-wave emissions can be used as an indicator of ULPE completeness, opening for the first time a way of in-situ monitoring of the process.

The application of ultrasound and acoustic cavitation in liquid exfoliation of bulk layered materials is a widely used method. However, despite extensive research, the fundamental mechanisms remain far from being fully understood. A number of theories have been proposed to interpret the interactions between cavitation and bulk layered materials and hence to explain the mechanisms of ultrasound assisted exfoliation. Unfortunately, most of the research reported to date is ambiguous or inconclusive due to lack of direct real-time experimental evidence. In this paper, we report systematic work characterising cavitation emissions and observing the exfoliation of graphite in situ, in deionised water under the dynamic interaction with laser and ultrasound induced cavitation bubbles. Using ultra-high-speed optical imaging, we were able to determine the dynamic sequence of graphite exfoliation events on a time scale never reported before. Real-time observations also revealed that shock waves with a pressure magnitude up to 5 MPa and liquid-jets in the range of 80 ms−1, from transient cavitation bubble implosions, were essential for the initiation and propagation of the exfoliation process. On the other hand, bubble oscillations associated with stable cavitation were beneficial for promoting a gentler delamination of graphite layers.

Scaling up ultrasonic cavitation melt treatment (UST) requires effective flow management with minimised energy requirements. To this end, container dimensions leading to the resonance play a crucial role in amplifying pressure amplitude for cavitation. To quantify the importance of resonance length during the treatment of liquid aluminium, we used calibrated high-temperature cavitometers (in the range of 8–400 kHz), to measure and record the acoustic pressure profiles inside the cavitation-induced environment of liquid Al and deionized water (used as an analogue to Al) excited at 19.5 kHz. To achieve a comprehensive map of the acoustic pressure field, measurements were conducted at three different cavitometer positions relative to the vibrating sonotrode probe and for a number of resonant and non-resonant container lengths based on the speed of sound in the treated medium. The results showed that the resonance length affected the pressure magnitude in liquid Al in all cavitometer positions, while water showed no sensitivity to resonance length. An important practical application of UST in aluminium processing concerns grain refinement. For this reason, grain size analysis of UST-treated Al-Cu-Zr-Ti alloy was used as an indicator of the melt treatment efficiency. The result showed that the treatment in a resonance tank of  (the wavelength of sound in Al) gave the best structure refinement as compared to other tested lengths. The data given here contribute to the optimisation of the ultrasonic process in continuous casting, by providing an optimum value for the critical compartment (e.g. in a launder of direct-chill casting) dimension.

This study concerns the numerical simulation of two competing ultrasonic treatment (UST) strategies for microstructure refinement in the direct-chill (DC) casting of aluminium alloys. In the first, more conventional, case, the sonotrode vibrating at 17.3 kHz is immersed in the hop-top to treat the sump melt pool, in the second case, the sonotrode is inserted between baffles in the launder. It is known that microstructure refinement depends on the intensity of acoustic cavitation and the residence time of the treated fluid in the cavitation zone. The geometry, acoustic field intensity, induced flow velocities, and local temperature are factors which affect this treatment. The mathematical model developed in this work couples flow velocity, acoustics modified by cavitation, heat transfer, and solidification at the macroscale, with Lagrangian refiner particles, used to determine: (a) their residence time in the active zones, and (b) their eventual distribution in the sump as a function of the velocity field. This is the first attempt at using particle models as an efficient, though indirect, alternative to microstructure simulation, and the results indicate that UST in the launder, assisted with baffle separators, yields a more uniform distribution of refining particles, avoiding the strong acoustic streaming jet that, otherwise, accompanies hot-top treatment, and may lead to the strong segregation of refining particles. Experiments conducted in parallel to the numerical studies in this work appeared to support the results obtained in the simulation.

In this work, we study how ultrasonic cavitation melt treatment (UST) affects the temperature distribution, sump profile, and resulting microstructure in the direct-chill (DC) casting of an AA6008 aluminum alloy. Two 152 mm diameter billets were cast; one was treated with UST (UST-DC casting) in the hot top while the other was not (conventional DC casting). To investigate the temperature distribution, temperature was measured at multiple points in both billets. The sump profile was visualized by pouring Zn into the sump during casting. The microstructure was analyzed by measuring the grain size of as-cast billets. A numerical model of DC casting and UST-DC casting has been validated with the temperature measurements across the billets, and the experimental results agrees well with the numerical model. It is found that the sump profile quantification with thermocouple measurements is more accurate and less prone to interpretation than with Zn tracing. Numerical simulation results show that UST application in the hot top with sonotrode position at 20 mm above the graphite ring level depresses the liquidus isotherm but does not affect the solidus isotherm, resulting in a thinner transition region compared with conventional DC casting. Grain structure analysis verifies that structure refinement with UST has been achieved at the given sonotrode position. The strongest grain refinement was at the center of the billet with the average grain size 50% smaller than that without UST. The results are discussed in terms of the known mechanisms of UST, i.e. dendrite fragmentation and deagglomeration of nucleating substrates.

The application of cavitation-induced shock waves generated at low driving frequencies, known as power ultrasound, is essential for a wide range of fields, such as sonochemistry, lithotripsy, nanomaterials, emulsions and casting, to name but a few. In this paper, we present measurements of the shock wave pressures emitted by cavitating bubbles in water, under ultrasonic excitation produced by an immersed probe oscillating at 24 kHz. A broad-spectrum fibre-optic hydrophone calibrated in the range of 1–30 MHz was used for this purpose. Spectral analysis of the data reveals a consistent resonance peak at a very narrow range of frequencies (3.27–3.43 MHz). Results were confirmed using real-time analysis of high-speed recordings. By eliminating other possible sources, we propose that this new peak might be associated with shock wave emissions from collapsing bubbles. Spatial maps obtained by collating individual shock wave pressures highlight the effect of pressure shielding with increasing input power, attributed to a cloud of bubbles surrounding the probe. This work contributes towards the elucidation of the key properties of cavitation-driven shock waves and the underlying mechanisms, essential in controlling the effectiveness of the external processing conditions on various physical, chemical and biological systems.

The performance augmentation of pairs of vertical axis wind turbines (VAWTs) is known to be dependent on incident wind direction, turbine spacing and direction of rotation. Yet, there is a lack of robust numerical models investigating the impact of these parameters. In this study two-dimensional CFD simulations of an isolated VAWT and of co- and counter-rotating pairs of VAWTs were performed with the aim to determine turbine layouts that can increase the power output of VAWT farms. More than 11,500 h of simulations were conducted at a turbine diameter Reynolds number of 1.35 · 107. A mesh convergence study was conducted, investigating the influence of mesh size, domain size, azimuth increment, number of iterations per time step, and domain cell density. Results showed that mesh size, domain size, and azimuth increment proved to have the biggest impact on the converged results. For the configurations analysed, pairs of VAWTs exhibited a 15% increase in power output compared to operating in isolation, when the second rotor was spaced three turbine diameters downstream and at an angle of 60° to the wind direction. Furthermore, when three turbines were positioned in series, the power output was greater than a pair by an additional 3%.

Ultrasonic emulsification (USE) assisted by cavitation is an effective method to produce emulsion droplets. However, the role of gas bubbles in the USE process still remains unclear. Hence, in the present paper, high-speed camera observations of bubble evolution and emulsion droplets formation in oil and water were used to capture in real-time the emulsification process, while experiments with different gas concentrations were carried out to investigate the effect of gas bubbles on droplet size. The results show that at the interface of oil and water, gas bubbles with a radius larger than the resonance radius collapse and sink into the water phase, inducing (oil–water) blended liquid jets across bubbles to generate oil-in-water-in-oil (O/W/O) and water-in-oil (W/O) droplets in the oil phase and oil-in-water (O/W) droplets in the water phase, respectively. Gas bubbles with a radius smaller than the resonance radius at the interface always move towards the oil phase, accompanied with the generation of water droplets in the oil phase. In the oil phase, gas bubbles, which can attract bubbles nearby the interface, migrate to the interface of oil and water due to acoustic streaming, and generate numerous droplets. As for the gas bubbles in the water phase, those can break neighboring droplets into numerous finer ones during bubble oscillation. With the increase in gas content, more bubbles undergo chaotic oscillation, leading to smaller and more stable emulsion droplets, which explains the beneficial role of gas bubbles in USE. Violently oscillating microbubbles are, therefore, found to be the governing cavitation regime for emulsification process. These results provide new insights to the mechanisms of gas bubbles in oil–water emulsions, which may be useful towards the optimization of USE process in industry.

This work focuses on ultrasonic melt treatment (UST) in a launder upon pilot-scale direct chill (DC) casting of 152-mm-diameter billets from an AA6XXX alloy with Zr addition. Two casting temperatures (650°C and 665°C) were used to assess their effect on the resulting microstructure (grain size, particle size, and number density). Structure refinement results show the feasibility of UST in the DC casting launder. This is quantified through the corresponding reduction of grain size by around 50% in the billet center, or more towards the billet surface, reduction of the average Al3Zr particle size, and increase in the particle number density. A higher Al3Zr particle density was obtained when the alloy was cast at 665°C. Numerical simulation results and suggestions on how to improve the treatment quality of UST in DC casting launder are also provided.

One of the main applications of ultrasonic melt treatment is the grain refinement of aluminium alloys. Among several suggested mechanisms, the fragmentation of primary intermetallics by acoustic cavitation is regarded as very efficient. However, the physical process causing this fragmentation has received little attention and is not yet well understood. In this study, we evaluate the mechanical properties of primary Al3Zr intermetallics by nano-indentation experiments and correlate those with in-situ high-speed imaging (of up to 1 Mfps) of their fragmentation process by laser-induced cavitation (single bubble) and by acoustic cavitation (cloud of bubbles) in water. Intermetallic crystals were chemically extracted from an Al-3 wt% Zr alloy matrix. Mechanical properties such as hardness, elastic modulus and fracture toughness of the extracted intermetallics were determined using a geometrically fixed Berkovich nano-diamond and cube corner indenter, under ambient temperature conditions. The studied crystals were then exposed to the two cavitation conditions mentioned. Results demonstrated for the first time that the governing fragmentation mechanism of the studied intermetallics was due to the emitted shock waves from the collapsing bubbles. The fragmentation caused by a single bubble collapse was found to be almost instantaneous. On the other hand, sono-fragmentation studies revealed that the intermetallic crystal initially underwent low cycle fatigue loading, followed by catastrophic brittle failure due to propagating shock waves. The observed fragmentation mechanism was supported by fracture mechanics and pressure measurements using a calibrated fibre optic hydrophone. Results showed that the acoustic pressures produced from shock wave emissions in the case of a single bubble collapse, and responsible for instantaneous fragmentation of the intermetallics, were in the range of 20–40 MPa. Whereas, the shock pressure generated from the acoustic cavitation cloud collapses surged up to 1.6 MPa inducing fatigue stresses within the crystal leading to eventual fragmentation.

Liquid Phase Exfoliation (LPE) is an efficient method for graphene flake exfoliation and considered to be compatible with industrial production requirements. However, most of available LPE methods require the use of harmful and expensive solvents for chemical exfoliation prior to mechanical dispersion of the flakes, and therefore an additional step is needed to remove the contamination caused by the added chemicals, making the process complex, costly, unsafe and detrimental to the environment.

By studying the effects of key ultrasonic LPE parameters, our study demonstrates the possibility to control the production and quality of few-layer graphene flakes in pure water in a relatively short period of time. The driving frequency of an ultrasonic source, a higher acoustic cavitation intensity and uniform distribution of the cavitation events in the sonicated volume are the key parameters for controlling the thickness, surface area and production yield of few-layer graphene flakes. The results are discussed in the context of mechanical exfoliation. This opens a direction for developing LPE into a cost effective, clean, environmentally friendly, and scalable manufacturing process for the next generation of two-dimensional nanomaterials for industrial-scale applications.

Quantitative understanding of the interactions of ultrasonic waves with liquid and solidifying metals is essential for developing optimal processing strategies for ultrasound processing of metal alloys in the solidification processes. In this research, we used the synchrotron X-ray high-speed imaging facility at Beamline I12 of the Diamond Light Source, UK to study the dynamics of ultrasonic bubbles in a liquid Sn-30wt%Cu alloy. A new method based on the X-ray attenuation for a white X-ray beam was developed to extract quantitative information about the bubble clouds in the chaotic and quasi-static cavitation regions. Statistical analyses were made on the bubble size distribution, and velocity distribution. Such rich statistical data provide more quantitative information about the characteristics of ultrasonic bubble clouds and cavitation in opaque, high-temperature liquid metals.

The prediction of the acoustic pressure field and associated streaming is of paramount importance to ultrasonic melt processing. Hence, the last decade has witnessed the emergence of various numerical models for predicting acoustic pressures and velocity fields in liquid metals subject to ultrasonic excitation at large amplitudes. This paper summarizes recent research, arguably the state of the art, and suggests best practice guidelines in acoustic cavitation modelling as applied to aluminium melts. We also present the remaining challenges that are to be addressed to pave the way for a reliable and complete working numerical package that can assist in scaling up this promising technology.

Acoustic streaming and its attendant effects in the sump of a direct-chill (DC) casting process are successfully predicted under ultrasonic treatment for the first time. The proposed numerical model couples acoustic cavitation, fluid flow, heat and species transfer, and solidification to predict the flow pattern, acoustic pressure, and temperature fields in the sump. The model is numerically stable with time steps of the order of 0.01 s and therefore computationally attractive for optimization studies necessitating simulation times of the order of a minute. The sump profile is altered by acoustic streaming, with the slurry region depressed along the centreline of the billet by a strong central jet. The temperature gradient in the transition zone is increased, potentially interfering with grain refinement. The cooling rate in the sump is also altered, thereby modifying the dendrite arm spacing of the as-cast billet. The relative position of the sonotrode affects the sump profile, with the sump depth decreased by around 5 mm when the sonotrode is moved above the graphite ring level by 100 mm. The acoustic streaming jet penetrates into the slurry zone and, as a result, the growth direction of dendritic grains in the off-centre position is altered.

The acoustic streaming behaviour below an ultrasonic sonotrode in water was predicted by numerical simulation and validated by experimental studies. The flow was calculated by solving the transient Reynolds-Averaged Navier-Stokes equations with a source term representing ultrasonic excitation implemented from the predictions of a nonlinear acoustic model. Comparisons with the measured flow field from Particle Image Velocimetry (PIV) water experiments revealed good agreement in both velocity magnitude and direction at two power settings, supporting the validity of the model for acoustic streaming in the presence of cavitating bubbles. Turbulent features measured by PIV were also recovered by the model. The model was then applied to the technologically important area of ultrasonic treatment of liquid aluminium, to achieve the prediction of acoustic streaming for the very first time that accounts for nonlinear pressure propagation in the presence of acoustic cavitation in the melt. Simulations show a strong dependence of the acoustic streaming flow direction on the cavitating bubble volume fraction, reflecting PIV observations. This has implications for the technological use of ultrasound in liquid metal processing.

Hydraulic components are coated by thermal spraying to protect them against cavitation erosion. These coatings are built up by successive deposition of single splats. The behavior of a single splat under mechanical loading is still very vaguely understood. Yttria-stabilized zirconia (YSZ) and stainless-steel splats were obtained by plasma spraying onto stainless steel substrates. The velocity and temperature of particles upon impact were measured and the samples were subsequently exposed to cavitation erosion tests. An acoustic cavitation simulation estimated the water jet velocity and hammer stresses exerted by bubble collapse on the surface of the specimen. Although the results suggested that high stress levels resulted from cavitation loading, it was clear that weak adhesion interfaces played a crucial role in the accelerated cavitation-induced degradation.

Ultrasonic (cavitation) melt processing attracts considerable interest from both academic and industrial communities as a promising route to provide clean, environment friendly and energy efficient solutions for some of the core issues of the metal casting industry, such as improving melt quality and providing structure refinement. In the last 5 years, the authors undertook an extensive research programme into fundamental mechanisms of cavitation melt processing using state-of-the-art and unique facilities and methodologies. This overview summarises the recent results on the evaluation of acoustic pressure and melt flows in the treated melt, direct observations and quantitative analysis of cavitation in liquid aluminium alloys, in-situ and ex-situ studies of the nucleation, growth and fragmentation of intermetallics, and de-agglomeration of particles. These results provide valuable new insights and knowledge that are essential for upscaling ultrasonic melt processing to industrial level.

This allowed quantification of not only the cavitation bubble formation and collapse, but there was also evidence of the previously hypothesised ultrasonic capillary effect (UCE), providing the first direct observations of this phenomenon in a molten metallic alloy. This was achieved by quantifying the re-filling of a pre-existing groove in the shape of a tube (which acted as a micro-capillary channel) formed by the oxide envelope of the liquid sample. Analytical solutions of the flow suggest that the filling process, which took place in very small timescales, was related to micro-jetting from the collapsing cavitation bubbles. In addition, a secondary mechanism of liquid penetration through the groove, which is related with the density distribution of the oxides inside the groove, and practically to the filtration of aluminium melt from oxides, was revealed. The observation of the almost instantaneous re-filling of a micro-capillary channel with the metallic melt supports the hypothesised sono-capillary effect in technologically important liquids other than water, like metallic alloys with substantially higher surface tension and density.

In this study, an in situ synchrotron radiography experiment was performed to investigate bubble dynamics in an Al-10 wt.% Cu alloy under an external ultrasound field at 30 kHz. Radiographs with an exposure time of 78 ms were collected continuously during the sonication of molten alloys at temperatures of 660±10 °C. To the best of our knowledge, this is the first time that transient cavitation bubbles have been observed in liquid aluminium. Quantification of bubble parameters such as average size and time of collapse were evaluated from radiographs using advanced image analysis. Additionally, broadband noise associated with the acoustic emissions from shock waves of transient cavitation bubbles and estimation of the real-time acoustic pressure at the driving frequency were assessed using an advanced high-temperature cavitometer in separate bulk experiments.

Three liquid environments and four steel grades were utilised experimentally. The liquids used for the tests were distilled water, used as a reference liquid, and the two working fluids of the scroll expander a synthetic lubricant and a high molecular refrigerant. The steel grades were a high carbon (AISI 1085) and low carbon (AISI 1010) martensitic steel with retained austenite, a chromium martensitic steel (AISI 52100) and a martensitic scroll plate (SP) sample. An ultrasonic transducer was utilised to produce cavitation conditions using a 5 mm diameter probe. The comparison of the results revealed the most hostile liquid environment according to the morphology evaluation of the incubation pits. The cavitation mechanisms are discussed and the cavitation resistance of the steel grades is evaluated. The best performing steel material against cavitation is determined for the conditions described.