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

Lead Research Organisation: Oxford Brookes University
Department Name: Faculty of Tech, Design and Environment

Abstract

Abstracts are not currently available in GtR for all funded research. This is normally because the abstract was not required at the time of proposal submission, but may be because it included sensitive information such as personal details.

Publications

10 25 50
 
Description The focus of this project is on finding a technological way of producing graphene and few-layer graphene using ecological solutions. Therefore, we use pure water and ultrasonic vibrations for exfoliation and dispersion of graphene flakes. So far we have produced graphene of quality and size comparable with the best published results of other research groups worldwide, while having used only water and rather short treatment times. The optimisation of process parameters is the key of success. The mechanisms of ultrasonic exfoliation are under scrutiny using the most advanced characterisation techniques and unique in-situ observations. It is demonstrated that the use of two ultrasonic sources with low (20 kHz) and high (1 MHz) frequencies facilitates the exfoliation and improves the quality of graphene flakes. Unique acoustic measurements have been made to explain the mechanism of dual frequency exfoliation. In-situ studies using optical and X-ray high-speed imaging revealed a number of previously unknown mechanisms of cavitation-induced exfoliation, which are also supported by numerical modelling and acoustic measurements. An important role of shock-waved emitted upon cavitation has been revealed and quantified. A new acoustic signature of exfoliation has been identified (MHz-frequency peak) that can be potentially used for monitoring the exfoliation accomplishment. A number of high-ranking papers have been published and more are in preparation. The results have been reported at a number of important international conferences. Current efforts are focused on further improvement of the exfoliation yield (>10%) and quality (less than 8 layers, size large than 1 µm) by a combination of green and eco-friendly solvents and surfactants with promising results starting to emerge. Also the first steps towards testing and functionalisation of graphene flakes have started by Greenwich university.

Unfortunately the planned contribution of Oxford/Greenwich partners has not been realised to a full measure. Multiple issues in communication, access to the equipment, references to the lack of time and other difficulties prevented the consortium from using Oxford experiments and facilities to the planned extent. As a result, only one paper has originated based on the results of this team. Brunel and Oxford Brookes Universities had, therefore, extra work carried out. A follow-up grant proposal has not been supported by EPSRC despite excellent reviews (see Narrative Impact), which is a great disappointment.
Exploitation Route A number of high-impact journal publications are published and in preparation. The results have been reported at a number of international conferences.
Sectors Chemicals,Energy,Manufacturing, including Industrial Biotechology,Pharmaceuticals and Medical Biotechnology

 
Description It is shown that a combination of low- and high frequency ultrasonic sources gives a synergetic effect in the efficiency of liquid-phase exfoliation of graphite. Acoustic measurements demonstrate the increase of acoustic pressure due to the use of two different-frequency sources. This allows us to use pure water free of polluting and harmful additions and considerably shorter processing times than has been reported before. A number of green/eco-friendly surfactants are used to increase the yield and quality of the 2D flakes by improving the separation and stability of produced mixtures. Advanced in situ observations and measurements provide insights into the previously uncharted mechanisms of mechanical exfoliation of graphite by cavitation bubbles of difference sizes as well as by acoustic flows. Optimisation of process parameters and upscaling of the process are underway by setting up a continuous recirculating-flow reactor. The main outcome is the development of a technology for eco-friendly production of graphene for medical (drag delivery and diagnostics) and environmental (water purification) applications that is now tested with FORTH (Greece). A highly rated research proposal (EcoCavActor; grades 6, 5, 5) submitted to EPSRC in 2021 and aimed at upscaling the results of this research has eventually not been supported by EPSRC (even if EPSRC was very keen to fund this project, it is held for 4 consecutive engineering prioritisation meetings, unfortunately EPSRC did not have enough budget to support this proposal) and other routes will be pursued in this direction. In line with this and based on the outcomes of the EcoUltra2D project that set the scene a recent research proposal was funded from the Royal Society (International Newton Fund Award; NIF\R1\221238) where a new approach is proposed for eco-friendly graphene and other 2Ds production at large scale.
First Year Of Impact 2023
Sector Chemicals,Energy,Manufacturing, including Industrial Biotechology,Pharmaceuticals and Medical Biotechnology
Impact Types Economic

 
Description Ultra-high speed camera observations 
Organisation University of Glasgow
Country United Kingdom 
Sector Academic/University 
PI Contribution We have identify for the first time using advanced camera observations the prime responsible mechanisms for the sono-exfoliation of graphite in water
Collaborator Contribution Allowed us to use their state of the art facility providing knowledge and expertise
Impact a number of outputs is under development; more experiments are scheduled for this year
Start Year 2019
 
Description ESS-JSS-AOSS 1st JOINT SONOCHEMISTRY CONFERENCE (ONLINE) 
Form Of Engagement Activity Participation in an activity, workshop or similar
Part Of Official Scheme? No
Geographic Reach International
Primary Audience Professional Practitioners
Results and Impact Two presentations at this major Sonochemistry event
Year(s) Of Engagement Activity 2021
 
Description Graphene 2021 
Form Of Engagement Activity Participation in an activity, workshop or similar
Part Of Official Scheme? No
Geographic Reach International
Primary Audience Industry/Business
Results and Impact Two presentations at the major event on graphene science and technology: Graphene 2021 (October 26-29, 2021 Grenoble (France))
Year(s) Of Engagement Activity 2021
 
Description Invited talk at the 2D symposium within TMS 2023 
Form Of Engagement Activity Participation in an activity, workshop or similar
Part Of Official Scheme? No
Geographic Reach International
Primary Audience Professional Practitioners
Results and Impact Invited talk at the Symposium on 2D Materials (TMS Annual Meeting, San Diego, March 2023)
Year(s) Of Engagement Activity 2022
 
Description Invited talk in the 184th Meeting of the Acoustical Society of America 
Form Of Engagement Activity Participation in an activity, workshop or similar
Part Of Official Scheme? No
Geographic Reach International
Primary Audience Professional Practitioners
Results and Impact An invited talk in the annual event of the Acoustical Society of America (Chicago, 8-12 May 2023).
Year(s) Of Engagement Activity 2022
 
Description Participation in CAV 2021 Symposium 
Form Of Engagement Activity Participation in an activity, workshop or similar
Part Of Official Scheme? No
Geographic Reach International
Primary Audience Professional Practitioners
Results and Impact One presentation on the 11th International Symposium on Cavitation 2021 (CAV2021), Virtual Conference from 10 to 13 May 2021 in Korea
Year(s) Of Engagement Activity 2021
 
Description Talk at TMS2022 2D materials 
Form Of Engagement Activity A talk or presentation
Part Of Official Scheme? No
Geographic Reach International
Primary Audience Industry/Business
Results and Impact A talk at the symposium 2D Materials - Preparation, Properties & Applications within the TMS 2022 Annual Meeting in Anaheim, USA
Year(s) Of Engagement Activity 2022