Sustainable and industrially scalable ultrasonic liquid phase exfoliation technologies for manufacturing 2D advanced functional materials (EcoUltra2D)

Lead Research Organisation: University of Hull
Department Name: Mechanical Engineering

Abstract

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Publications

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Eskin DG (2019) Fundamental studies of ultrasonic melt processing. in Ultrasonics sonochemistry

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Khavari M (2023) Cavitation-induced shock wave behaviour in different liquids in Ultrasonics Sonochemistry

 
Description In this report period, we are able to compete two most important MHz real-time imaging of ultrasonic exfoliation of different 2D functional materials. One at the European XFEL in Sept 2022 and the other at the Advanced Photon Source in Dec 2022. The experiments are the world first attempt on using MHz X-ray imaging to study at sub-µs and µm scale the liquid exfoliation dynamics.
Approximately 10 TB real-time image data were collected and 50% of them are now analysed. The very rich data allow us to fully validate and optimise the multiphysics numerical models. Experimental and modelling results clearly reveal that
(1) Ultrasonic cavitation bubbles implosion occurs in a few ultrasound cycles. At implosion, shock waves with a velocity of ~120 m/s are emitted and acting on the 2D materials. The interactions impose cyclic impulsive forces onto the layer materials and they are the main driving forces for initiating surface defects, expanding interlayer spacing and progressively exfoliating thin graphite bundles into large graphite layers by the continuous fatigue effect.

(2) The exfoliation rate and efficiency were largely determined by the size of the effective cavitation zone and the cavitation bubble number density for generating sufficient implosion events for exfoliation. The size of the cavitation zone is predominantly affected by the input acoustic pressure field, the geometry of the sonotrode wave emitting surface, and the properties of the solvents.

(3) Outside the cavitation bubble zone, the efficiency of exfoliation decreased significantly and simply increasing the sonication time did not have much effect on increasing the exfoliation efficiency. These findings have guided the design of up-scale ultrasound liquid exfoliation experiment apparatus and the optimisation of the semi-continuous operation for producing sufficient quantities of 2D materials at other partner universities.
Exploitation Route The enhanced exfoliation process due to the shock wave produced at ultrasonic bubble implosion is significant for the manufacture of 2D layer materials. It has the potential to increase significantly the production rate of 2D layer materials, for example, graphene, MoS2, WS2, h-BN, h-BCN, etc.
Sectors Aerospace, Defence and Marine,Agriculture, Food and Drink,Chemicals,Energy,Healthcare,Manufacturing, including Industrial Biotechology,Pharmaceuticals and Medical Biotechnology

URL https://www.hull.ac.uk/work-with-us/research/groups/advanced-materials-and-acoustics
 
Description The key findings from the real-time and operando studies as well as the optimisation strategies from the modelling have informed and guided other tasks undertaken by Brunel, Oxford, Oxford Brookes universities for their work on upscaling of the ultrasonic exfoliation process and the relevant optimisation production of 2D materials, especially for the continuous recirculating-flow reactor and the high intensive shear reactor.
First Year Of Impact 2022
Sector Energy,Environment
 
Description Sustainable and industrially scalable ultrasonic liquid phase exfoliation technologies for manufacturing 2D advanced functional materials (EcoUltra2D)
Amount £330,623 (GBP)
Funding ID EP/R031819/1 
Organisation Engineering and Physical Sciences Research Council (EPSRC) 
Sector Public
Country United Kingdom
Start 09/2018 
End 09/2021
 
Title Data and videos for ultrafast synchrotron X-ray imaging studies of metal solidification under ultrasound 
Description The data presented in this article are related to the paper entitled 'Ultrafast synchrotron X-ray imaging studies of microstructure fragmentation in solidification under ultrasound' [Wang et al., Acta Mater. 144 (2018) 505-515]. This data article provides further supporting information and analytical methods, including the data from both experimental and numerical simulation, as well as the Matlab code for processing the X-ray images. Six videos constructed from the processed synchrotron X-ray images are also provided. 
Type Of Material Database/Collection of data 
Year Produced 2018 
Provided To Others? Yes  
Impact These are a set of high speed X-ray image data and the relevant numerical simulation results (including the Matlab code used for processing the X-ray images) made available for the researchers and engineers to understand the multi-physics and multi-length scale phenomena in ultrasound materials processing. The information is valuable for modelling and simulation validation and developing the optimization strategy for ultrasound melt processing in industry. 
URL https://www.sciencedirect.com/science/article/pii/S2352340918301148?via%3Dihub
 
Description Established a collaborative research consortium with Cranfield University 
Organisation Cranfield University
Country United Kingdom 
Sector Academic/University 
PI Contribution In the past 2 years or so, my team at University of Hull collaborated with the research team at the Sustainable Manufacturing Systems Centre of Cranfield University and formed a research consortium with Brunel University and industry partners to bid for the EPSRC funding call "Sustainable manufacturing, 15 July 2021". My team is responsible for developing low-energy and sustainable external field-based melt processing technology for recycled aluminium alloys.
Collaborator Contribution The Cranfield team is responsible for developing digital network-enabled transformation technologies and circular economy-based business model for the casting industry to manufacture aluminium based materials for the low carbon economy.
Impact So far there is no publication output yet.
Start Year 2020
 
Description Linked projects with Oxford University (EP/R031975/1), Brunel University (EP/R031665/1), and Oxford Brooks University (EP/R031401/1) 
Organisation Brunel University London
Department Brunel Centre for Advanced Solidification Technology (BCAST)
Country United Kingdom 
Sector Academic/University 
PI Contribution This is research consortium, my team at University of Hull is mainly responsible for studying the fundamental mechanisms of ultrasonic liquid exfoliation using advanced modelling and ultrafast synchrotron X-ray imaging method.
Collaborator Contribution The team at University of Oxford is mainly responsible for characterising and testing of the exfoliated 2D materials The team at Brunel University is mainly responsible for developing and optimising sono-exfoliation techniques for graphene and other 2D materials. The team at Oxford Brooks University is mainly responsible for designing new processing reactor, and the production of 2D nanomaterials
Impact Three joint journal publicaitons are currently under review.
Start Year 2017
 
Description Linked projects with Oxford University (EP/R031975/1), Brunel University (EP/R031665/1), and Oxford Brooks University (EP/R031401/1) 
Organisation Oxford Brookes University
Country United Kingdom 
Sector Academic/University 
PI Contribution This is research consortium, my team at University of Hull is mainly responsible for studying the fundamental mechanisms of ultrasonic liquid exfoliation using advanced modelling and ultrafast synchrotron X-ray imaging method.
Collaborator Contribution The team at University of Oxford is mainly responsible for characterising and testing of the exfoliated 2D materials The team at Brunel University is mainly responsible for developing and optimising sono-exfoliation techniques for graphene and other 2D materials. The team at Oxford Brooks University is mainly responsible for designing new processing reactor, and the production of 2D nanomaterials
Impact Three joint journal publicaitons are currently under review.
Start Year 2017
 
Description Linked projects with Oxford University (EP/R031975/1), Brunel University (EP/R031665/1), and Oxford Brooks University (EP/R031401/1) 
Organisation University of Oxford
Department Department of Materials
Country United Kingdom 
Sector Academic/University 
PI Contribution This is research consortium, my team at University of Hull is mainly responsible for studying the fundamental mechanisms of ultrasonic liquid exfoliation using advanced modelling and ultrafast synchrotron X-ray imaging method.
Collaborator Contribution The team at University of Oxford is mainly responsible for characterising and testing of the exfoliated 2D materials The team at Brunel University is mainly responsible for developing and optimising sono-exfoliation techniques for graphene and other 2D materials. The team at Oxford Brooks University is mainly responsible for designing new processing reactor, and the production of 2D nanomaterials
Impact Three joint journal publicaitons are currently under review.
Start Year 2017
 
Description Megahertz Imaging of Ultrasonic Exfoliation of 2D Functional Materials 
Organisation European XFEL
Country Germany 
Sector Academic/University 
PI Contribution This research partnership involves the research teams from University of Hull, the European XFEL, DESY and Lund University Sweden. We jointly won the XFEL's first official MHz imaging beamtime experiment via the proposal "Megahertz Imaging the Implosion of Ultrasonic Bubbles and Their Effects on Exfoliation of 2D Functional Materials". The experiment was conducted at the SPB/SFX beamline of the EU XFEL on 10-19 September 2022. Myself and my team from the University of Hull provides the scientific research case, i.e., ultrasonic exfoliation of 2D functional materials, and the relevant materials and in-situ study equipment
Collaborator Contribution The team at SPB/SFX beamline of the EU XFEL and that of DESY provide the MHz imaging capability and technical support in executing the experiment. The research team of Lund University provides support in data reduction and processing.
Impact Approximately 7TB MHz imaging data were collected in September 2022 and then fully analyzed in the next 3-4 months. The results clearly reveal and elucidate the underlying mechanisms of how ultrasonic bubble implosion and the associated shock wave in facilitating layer exfoliation of 2D materials. Parts of the results have been presented by Professor Jiawei Mi in an invited plenary speech at the Annual EuXFEL User Meeting on 25-27 Jan 2023, which was well-received by the scientific community.
Start Year 2020