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
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People |
ORCID iD |
| Iakovos Tzanakis (Principal Investigator) |
Publications
Eskin D
(2023)
Sonoprocessing of materials (Special issue).
in Ultrasonics sonochemistry
Kaur A
(2022)
Temperature as a key parameter for graphene sono-exfoliation in water.
in Ultrasonics sonochemistry
Khavari M
(2021)
Scale up design study on process vessel dimensions for ultrasonic processing of water and liquid aluminium.
in Ultrasonics sonochemistry
Khavari M
(2021)
Characterization of shock waves in power ultrasound
in Journal of Fluid Mechanics
Khavari M
(2023)
Cavitation-induced shock wave behaviour in different liquids.
in Ultrasonics sonochemistry
Morton J
(2021)
New insights into sono-exfoliation mechanisms of graphite: In situ high-speed imaging studies and acoustic measurements
in Materials Today
Morton J
(2023)
Dual frequency ultrasonic cavitation in various liquids: High-speed imaging and acoustic pressure measurements
in Physics of Fluids
Morton J
(2022)
An Eco-Friendly Solution for Liquid Phase Exfoliation of Graphite Under Optimised Ultrasonication Conditions
in SSRN Electronic Journal
| 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. The principal role of shockwaves emitted upon collapse of cavitation bubbles has been established. 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 towards fabrication of eco-graphene based electrodes for fuel cell applications. 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. Despite receiving excellent reviews, a follow-up grant proposal was not supported by EPSRC, which was a great disappointment. However, the results sparked the interest of many institutes worldwide, and eventually, collaboration with Sabanci University in Turkey led to a successful grant from the Royal Society in 2023 through the Isaac Newton International Fellowships award. This grant is aimed at scaling up our eco-friendly approach using a combination of hydrodynamic and acoustic cavitation. |
| 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 Environment 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. The optimization of process parameters and control of cavitation dynamics, along with the upscaling of the process, have been successful through the implementation of a continuous recirculating-flow reactor. The main outcome is the development of a technology for eco-friendly production of graphene for medical (drug delivery and diagnostics) and environmental (water purification) applications, which is currently being tested with FORTH (Greece) and the Faculty of Health Sciences, Biomedical Science (BMS), at Oxford Brookes University. Additionally, collaborations include solar cell fabrication with HMU (Greece) and carbon fiber production in partnership with Imperial College. A highly rated research proposal (EcoCavActor; grades 6, 5, 5) was submitted to EPSRC in 2021 with the aim of upscaling the results of this research. Unfortunately, despite EPSRC's keen interest in funding the project, it was held for four consecutive engineering prioritization meetings due to budget constraints. Regrettably, EPSRC was unable to allocate sufficient budget to support this proposal. Alternative routes were pursued in this direction. Subsequently, based on the outcomes of the EcoUltra2D project that set the scene, a research proposal was funded by the Royal Society (International Newton Fund Award; NIF\R1\221238), where a new approach is proposed for eco-friendly graphene and other 2D materials production at large scale utilising hybrid acoustic and hydrodynamic cavitation technologies. |
| First Year Of Impact | 2021 |
| Sector | Chemicals,Energy,Environment,Manufacturing, including Industrial Biotechology,Pharmaceuticals and Medical Biotechnology |
| Impact Types | Societal Economic |
| Description | Large Scale Exfoliation of 2D nanomaterials using an Environmentally Friendly Hybrid Cavitation Reactor |
| Amount | £145,000 (GBP) |
| Funding ID | NIF\R1\221238 |
| Organisation | The Royal Society |
| Sector | Charity/Non Profit |
| Country | United Kingdom |
| Start | 03/2023 |
| End | 03/2025 |
| Title | Signal Processing Matlab code |
| Description | Develop an in-house Matlab code to process acoustic signals from a range of calibrated to NPL sensors. This was proven instrumental for data processing and analysis, numerical model optimazation and succesful completion of a number of journal papers. |
| Type Of Material | Improvements to research infrastructure |
| Year Produced | 2021 |
| Provided To Others? | Yes |
| Impact | Without this tool we wouldn't be able to process the collected data and thus generate meaningful results. Also this tool is free to download from the http://cav-it.co.uk/ (website under development) and use for research or teaching purposes. |
| Description | Collaboration with FORTH (Greece) regarding cytotoxicity assessment of bio-friendly Graphene flakes for nanocarrier applications via NFFA call (Horizon, ID:184) |
| Organisation | Foundation for Research and Technology Hellas (FORTH) |
| Country | Greece |
| Sector | Public |
| PI Contribution | Ultrasonic liquid phase exfoliation of graphite in Phosphate Buffer Saline (PBS) yielded graphene flakes, which were assessed for cytotoxicity on mouse fibroblasts NIH-3T3 cells in FORTH and in human cells at OBU's Faculty of Health Sciences, Biomedical Science (BMS). The study aimed to evaluate the potential of bio-friendly graphene nanocarriers for targeted drug delivery in oncology, showing promising results with low cytotoxicity in fibroblast and human cells RPE-1 cells and higher efficacy in He-La cancer cells. |
| Collaborator Contribution | FORTH: Tested graphene with fibroblasts using standard protocols and procedures including nonlinear microscopy, live cell imaging, scanning electron microscopy and cell culture facilities BMS: Tested graphene with human and cancer cells using standard protocols and procedures involving calorimetric MTT assays |
| Impact | A manuscript on aqueous graphene's viability and morphology is due for submission The Post-doc working in this project has also submitted in 2023 a Dorothy Hodgkin (DH-2023/24) eight-year grant application to The Royal Society entitled "Eco-Graphene, a promising bio-compatible nanocarrier from nanotechnology to nano-oncology" to investigate the potential of bio-friendly grapehene nanocarriers in stimuli-responsive targeted drug delivery A follow up NFFA Horizon proposal (ID: 521) has been submitted and accepted with further tests scheduled for summer 2024 in the FORTH facilities An EPSRC proposal based on nanoengineering and functionalization of grapehne nanocarriers for gene transport and vaccine development between Brunel and Oxford Brookes supported by FORTH, involving biomedical departments from both universities, is in the early stages |
| Start Year | 2022 |
| Description | Collaboration with HMU (Greece) regarding integration of our eco-friendly graphene product into perovskite solar cell (PSC) device fabrication via EMERGE call (Horizon, ID:5816) |
| Organisation | Hellenic Mediterranean University |
| Department | Department of Electronic Engineering |
| Country | Greece |
| Sector | Academic/University |
| PI Contribution | Graphene inks (0.5 mg/ml) in eco-friendly solvents water, water-ethanol and water-IPA were produced with ULPE technique in Oxford Brookes |
| Collaborator Contribution | Inks were then deposited on glass and flexible PET substrates using spray/spin and slot-die coating techniques to create graphene films (20 mm x 15 mm) at HMU. Films were tested for electrical conductivity and other electrical properties |
| Impact | The resultant graphene films developed were homogenous with a thickness of 70 nm (RMS roughness 5 nm) and highly conductive (16 S/m), making them an excellent option for use as an interlayer on top of the electron transport layer (ETL) in the production of the highly promising perovskite solar cell (PSC) devices. |
| Start Year | 2023 |
| Description | Collaboration with Imperial College (Prof. Shaffer and Dr. Brandt-Talbot) for the production of carbon fibres from lignin/graphene dopes |
| Organisation | Imperial College London |
| Country | United Kingdom |
| Sector | Academic/University |
| PI Contribution | We developed lignin/graphene dopes (12 wt. % lignin+0.5 wt. % graphene) and graphene dispersions in appropriate water/ethanol/ionic liquid ratios (0.5 wt.%) with our novel ultrasonic technique developed in the EcoUltra2D project. |
| Collaborator Contribution | Studies on solubility, rheology and wet-spinning of obtained dopes were carried out at Imperial College London. |
| Impact | We have obtained carbon fibres from lignin/graphene dopes; the obtained fibres were fragile with coagulation of small fibres (of length 1-2 cm); next step is tailoring of the dope composition with improved graphene concentration to produce robust fibres |
| Start Year | 2023 |
| 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 | Editing a Special Issue of Ultrasonics Sonochemistry |
| Form Of Engagement Activity | A magazine, newsletter or online publication |
| Part Of Official Scheme? | No |
| Geographic Reach | International |
| Primary Audience | Professional Practitioners |
| Results and Impact | A Special Issue on Sonoprocessing of Materials was launched from the Journal of Ultrasonics Sonochemistry (IF 9.336) with Guest Editors Professor Dmitry Eskin (Brunel London University, UK), Professor Iakovos Tzanakis (Oxford Brookes University, UK) and Professor Sergey Komarov (Tohoku University, Japan). Special issue attracted a large number of papers (>50) on a wide range of topics with a view to establishing links and collaborations between scientists with complementary interests. |
| Year(s) Of Engagement Activity | 2022 |
| URL | https://www.journals.elsevier.com/ultrasonics-sonochemistry/call-for-papers/call-for-papers-on-speci... |
| 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 at the Institute of Physics (IoP) Group Tutorial Day (2023) in London - Acoustics in Action |
| Form Of Engagement Activity | Participation in an activity, workshop or similar |
| Part Of Official Scheme? | No |
| Geographic Reach | National |
| Primary Audience | Postgraduate students |
| Results and Impact | The tutorial day attracted a diverse audience mainly students (~30) from Imperial, Glasgow, Surrey, Oxford Brookes and Oxford Universities as well as academic professionals and industry representatives across the UK. On this tutorial day, novel applications, up-scaling and cavitation metrology were discussed which sparked questions and discussions afterwards, especially among PhD students and other Post-docs. |
| Year(s) Of Engagement Activity | 2023 |
| URL | https://iop.eventsair.com/pagtd2023/ |
| 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 | Invited talk in the ERC Workshop on Cavitation Exploitation in Ljubljana, Slovenia. |
| 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 | Iakovos was invited to present a talk at the ERC Workshop on Cavitation Exploitation in Ljubljana, Slovenia. The title of his presentation was 'Ultrasonic Cavitation Processing of Multi-functional Materials: Fundamentals and Applications.' His talk generated significant interest from the audience, especially towards the optimization and control of ultrasonic technologies |
| Year(s) Of Engagement Activity | 2023 |
| URL | https://www.matevzdular.com/workshop-2023/ |
| Description | Participation and talk in the 17th Meeting of the European Society of Sonochemistry |
| 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 in this major event, which sparked questions and discussions on the fundamentals of bubble dynamics and cavitation processes due to new insights/knowledge that was discovered in this project |
| 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 CAV2021 |
| 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 | A talk at the 11th International Symposium on Cavitation, May 10-13, 2021, Daejon, Korea |
| Year(s) Of Engagement Activity | 2021 |
| URL | http://cav2021.org/ |
| 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 |
| Description | World Conference on Carbon |
| 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 | We had 2 presentations regarding the exfoliation of graphene using our novel reactor in green solvents that sparked fruitful discussions and led to the collaboration with Imperial College and Prof. Milo Shaffer |
| Year(s) Of Engagement Activity | 2022 |
| URL | https://www.rsc.org/events/detail/73030/carbon-2022 |