Electron Microscopy for the Characterisation and Manipulation of Advanced Functional Materials and their Interfaces at the Nanoscale

Lead Research Organisation: University of St Andrews
Department Name: Chemistry

Abstract

In 2013 we successfully applied to enhance electron microscopy at St Andrews through the Capital for Great Technologies scheme. The purpose of this new facility is to provide state of the art capability to analyse and control functional materials at the nanoscale to underpin and drive forward critical Materials research in Energy Materials, Catalysis, Photonics, Metamaterials and Electronics. All elements of the facility are well used and usage is expanding now that the new facilities have come on stream. Going forward, however, we are severely constrained by lack of facility operators. It is easy to project doubling or more of usage with a second skilled operator on the Scios and Titan in particular. Not only would this involve more operator time on the instruments, it would increase training time and afford more time for detailed studies.

Thus the purpose of this application is to secure the appointment of a second skilled operator for two years to increase productivity and indeed capability through more rounded coverage. This will minimise down time due to holidays, allow more than one of the key facilities to be operated by our specialists for research and/or training at a single time and most importantly will provide the space to train more users to a higher standard.

We also propose to increase the outreach of our facility in the region, holding two focused workshops and linking more strongly to Universities in our region. We also hope to link with the other major Materials Electron Microscopy Centre in Scotland to coordinate capabilities.

An improved web-based booking system will be implemented.

Planned Impact

Advanced materials underpin most of modern civilisation and touch every aspect of our lives from communications to healthcare. Advances in materials performance and especially materials architectures have enabled the great advances in communications and information technologies that have so dramatically impacted upon our daily lives. Clearly, advances in materials and materials structures will strongly enable the next generation of technologies from communications to healthcare and hence deliver significant impact by changing how we live as well as providing key growth opportunities for knowledge-based industries.

The increased usage of the Electron microscopy facility will not just benefit academic users at St Andrews, but will also greatly benefit our industry partners. We will also be to train more industry users to use our facilities, especially those co-located on the St Andrews campus.

The group at St Andrews has built its reputation in the more fundamental aspects of materials research; however St Andrews has increasingly recognised the need for translation of its findings into real applications. This been addressed by patents, licences, spin-outs and most importantly through co-location of Technology companies in the University. There now exists a strong engagement with a number of industrial partners involved in the development of new energy devices and functional materials. An important emerging opportunity to transition our technologies relates to development of a new Innovation Park ideally suited to prototyping and scale up. In 2011, the University purchased the 36 acre former Guardbridge Paper Mill to develop an Energy Centre based around biomass feedstock. The Energy Centre will only require a small part of the Guardbridge 36 acre site so it has opened up a unique opportunity to provide facilities for universities and businesses to demonstrate, test and develop prototypes at proof of concept stage before manufacture. It has the ability to become an "innovation bridge", mainly re-using the former mill buildings, thus achieving further carbon savings by avoiding the need to build new facilities.

Publications

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Desai AV (2023) Surface-Functionalized Metal-Organic Frameworks for Binding Coronavirus Proteins. in ACS applied materials & interfaces

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Desai AV (2023) Azo-functionalised metal-organic framework for charge storage in sodium-ion batteries. in Chemical communications (Cambridge, England)

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Gil MP (2023) Detecting emerald green in 19thC book bindings using vis-NIR spectroscopy. in Analytical methods : advancing methods and applications

 
Description This award has allowed detailed structural studies on a range of materials with important catalytic and electrochemical function. In particular it is supporting batteries and fuel cell research.
Exploitation Route This is a shared facility with wide access to others within St Andrews, other Universities and to Industry laboratories. Thefacility ios a strong enabler for industry engagement with a significant degree of industry usage
Sectors Chemicals,Energy,Environment

URL http://chemistry.st-and.ac.uk/em/
 
Description With a second operator significantly better utilisation of the facility has been delivered. More users, more companies and better research has been enabled. Importnat work has been performed on exsolution chemistry showing new mechanisms and new transition elements being exsoluted.
First Year Of Impact 2019
Sector Aerospace, Defence and Marine,Chemicals,Electronics,Energy
 
Title Electron microscopy characterisation 
Description Raman spectroscopy coupled with optical (light) microscopy. Tungsten filament SEM: user-friendly, low cost & high throughput, an ideal workhorse instrument. Field emission gun (FEG) SEM: high resolution & stability and soft X-ray emission spectrometer (SXES) for light element detection. Electron probe micro-analyser (EPMA): high precision compositional measurement, including light elements. 
Type Of Material Improvements to research infrastructure 
Year Produced 2021 
Provided To Others? Yes  
Impact Increased industrial and external engagement. Promotion of interdisciplinary collaboration. 
URL https://e-microscopy.wp.st-andrews.ac.uk/
 
Title Atomic-scale imaging of emergent order at a magnetic-field induced Lifshitz transition (dataset) 
Description  
Type Of Material Database/Collection of data 
Year Produced 2022 
Provided To Others? Yes  
URL https://risweb.st-andrews.ac.uk/portal/en/datasets/atomicscale-imaging-of-emergent-order-at-a-magnet...
 
Title Azo-Functionalised Metal-Organic Framework for Charge Storage in Sodium-ion Batteries (dataset) 
Description  
Type Of Material Database/Collection of data 
Year Produced 2023 
Provided To Others? Yes  
URL https://risweb.st-andrews.ac.uk/portal/en/datasets/azofunctionalised-metalorganic-framework-for-char...
 
Title Batch and Bulk Adsorptive Removal of Anionic Dye using Metal/Halide-Free Ordered Mesoporous Carbon as Adsorbent (dataset) 
Description  
Type Of Material Database/Collection of data 
Year Produced 2022 
Provided To Others? Yes  
URL https://risweb.st-andrews.ac.uk/portal/en/datasets/batch-and-bulk-adsorptive-removal-of-anionic-dye-...
 
Title CCDC 2151572: Experimental Crystal Structure Determination 
Description Related Article: Pia S. Klee, Yuri Hirano, David B. Cordes, Alexandra M. Z. Slawin, Julia L. Payne|2022|Cryst.Growth Des.|22|3815|doi:10.1021/acs.cgd.2c00187 
Type Of Material Database/Collection of data 
Year Produced 2022 
Provided To Others? Yes  
URL http://www.ccdc.cam.ac.uk/services/structure_request?id=doi:10.5517/ccdc.csd.cc2b6wk0&sid=DataCite
 
Title Constitutionally selective dynamic covalent nanoparticle assembly (dataset) 
Description  
Type Of Material Database/Collection of data 
Year Produced 2022 
Provided To Others? Yes  
URL https://risweb.st-andrews.ac.uk/portal/en/datasets/constitutionally-selective-dynamic-covalent-nanop...
 
Title Coordination-Controlled Electrodeposition of Palladium/Copper Thin Films onto a Pyridine-Terminated Self-Assembled Monolayer (dataset) 
Description  
Type Of Material Database/Collection of data 
Year Produced 2022 
Provided To Others? Yes  
URL https://risweb.st-andrews.ac.uk/portal/en/datasets/coordinationcontrolled-electrodeposition-of-palla...
 
Title Data underpinning Influence of Electrode Processing and Electrolyte Composition on Multiwall Carbon Nanotube Negative Electrodes for Sodium Ion Batteries 
Description  
Type Of Material Database/Collection of data 
Year Produced 2023 
Provided To Others? Yes  
URL https://risweb.st-andrews.ac.uk/portal/en/datasets/data-underpinning-influence-of-electrode-processi...
 
Title Enhanced photoluminescence and reduced dimensionality via vacancy ordering in a 10H halide perovskite (dataset) 
Description  
Type Of Material Database/Collection of data 
Year Produced 2023 
Provided To Others? Yes  
URL https://risweb.st-andrews.ac.uk/portal/en/datasets/enhanced-photoluminescence-and-reduced-dimensiona...
 
Title Interplay of ferromagnetism and spin-orbit coupling in Sr4Ru3O10 (dataset) 
Description  
Type Of Material Database/Collection of data 
Year Produced 2022 
Provided To Others? Yes  
URL https://risweb.st-andrews.ac.uk/portal/en/datasets/interplay-of-ferromagnetism-and-spinorbit-couplin...
 
Title Mechanochemical synthesis of sodium carboxylates as anode materials in sodium ion batteries (dataset) 
Description Raw data 
Type Of Material Database/Collection of data 
Year Produced 2021 
Provided To Others? Yes  
URL https://risweb.st-andrews.ac.uk/portal/en/datasets/mechanochemical-synthesis-of-sodium-carboxylates-...
 
Title Multifaceted Study of the Interactions between CPO-27-Ni and Polyurethane and Their Impact on Nitric Oxide Release Performance (dataset) 
Description N/A 
Type Of Material Database/Collection of data 
Year Produced 2020 
Provided To Others? Yes  
Impact N/A 
URL https://risweb.st-andrews.ac.uk/portal/en/datasets/multifaceted-study-of-the-interactions-between-cp...
 
Title Ordered mesoporous carbons with body centred cubic pore structure (dataset) 
Description  
Type Of Material Database/Collection of data 
Year Produced 2022 
Provided To Others? Yes  
URL https://risweb.st-andrews.ac.uk/portal/en/datasets/ordered-mesoporous-carbons-with-body-centred-cubi...
 
Title Platinum incorporation into titanate perovskites to deliver emergent active and stable platinum nanoparticles (dataset) 
Description  
Type Of Material Database/Collection of data 
Year Produced 2021 
Provided To Others? Yes  
URL https://risweb.st-andrews.ac.uk/portal/en/datasets/platinum-incorporation-into-titanate-perovskites-...
 
Title Replacement of Ca by Ni in a Perovskite Titanate to Yield a Novel Perovskite Exsolution Architecture for Oxygen-Evolution Reactions (dataset) 
Description Supplementary Information 
Type Of Material Database/Collection of data 
Year Produced 2020 
Provided To Others? Yes  
URL https://risweb.st-andrews.ac.uk:443/portal/en/datasets/replacement-of-ca-by-ni-in-a-perovskite-titan...
 
Title Silicon Redistribution, Acid Site Loss and the Formation of a Core-Shell Texture upon Steaming SAPO-34 and their Impact on Catalytic Performance in the MTO Reaction (dataset) 
Description Effect of Steaming on SAPO34 
Type Of Material Database/Collection of data 
Year Produced 2020 
Provided To Others? Yes  
Impact Publication 
URL https://risweb.st-andrews.ac.uk/portal/en/datasets/silicon-redistribution-acid-site-loss-and-the-for...
 
Title Surface functionalized metal-organic frameworks for binding coronavirus proteins (dataset) 
Description  
Type Of Material Database/Collection of data 
Year Produced 2023 
Provided To Others? Yes  
URL https://risweb.st-andrews.ac.uk/portal/en/datasets/surface-functionalized-metalorganic-frameworks-fo...
 
Title Synthesis, structure and tunability of zero dimensional organic-inorganic metal halides utilising the m-xylylenediammonium cation: MXD2PbI6, MXDBiI5 and MXD3Bi2Br12ยท2H2O (dataset) 
Description The data files are not yet publicly available. Enquiries and requests for data should be directed to the publication's corresponding authors 
Type Of Material Database/Collection of data 
Year Produced 2022 
Provided To Others? Yes  
URL https://risweb.st-andrews.ac.uk/portal/en/datasets/synthesis-structure-and-tunability-of-zero-dimens...
 
Title Understanding the Anion-Templated, OSDA-Free, Interzeolite Conversion Synthesis of High Silica ZK-5 (dataset) 
Description  
Type Of Material Database/Collection of data 
Year Produced 2022 
Provided To Others? Yes  
URL https://risweb.st-andrews.ac.uk/portal/en/datasets/understanding-the-aniontemplated-osdafree-interze...
 
Title Use of interplay between A-site non-stoichiometry and hydroxide doping to deliver novel proton-conducting perovskite oxides (dataset) 
Description A draft for submission to a journal 
Type Of Material Database/Collection of data 
Year Produced 2021 
Provided To Others? Yes  
URL https://risweb.st-andrews.ac.uk/portal/en/datasets/use-of-interplay-between-asite-nonstoichiometry-a...
 
Title METHOD FOR PRODUCING AN ELECTRODE CATALYST FROM A PEROVSKITE METAL OXIDE 
Description The invention relates to a method of producing electrode materials for solid oxide cells which comprises applying an electric potential to a metal oxide which has a perovskite crystal structure. The resultant electrode catalyst exhibits excellent electrochemical performance. The invention extends to the electrode catalyst itself, and to electrodes and solid oxide cells comprising the electrode catalyst. 
IP Reference CA3030088 
Protection Patent application published
Year Protection Granted 2018
Licensed Commercial In Confidence
Impact -
 
Description ECECR2019 - Dr Aaron Naden 
Form Of Engagement Activity A talk or presentation
Part Of Official Scheme? No
Geographic Reach Regional
Primary Audience Professional Practitioners
Results and Impact Early career researcher conference: Awarded SCI prize for the best presentation (audience prize
Year(s) Of Engagement Activity 2019
 
Description EMRS, Virtual Conference 
Form Of Engagement Activity A talk or presentation
Part Of Official Scheme? No
Geographic Reach International
Primary Audience Professional Practitioners
Results and Impact The VIRTUAL 2021 Spring Meeting will consist of parallel symposia with invited speakers, oral and poster presentations, assorted by plenary sessions and a number of workshops and training courses. As a new item for posters, short oral presentation will give each attendee the opportunity to highlight the major results.

The high quality scientific program will address different topics organized into 19 symposia arranged in 4 clusters covering the fields of energy materials, nanomaterials and advanced characterization, biomaterials and soft materials, as well as materials for electronics, magnetics and photonics.

In parallel with the technical sessions, international exhibitors will have the opportunity to promote their equipment, systems, products, software, publications and services during the meeting.
Year(s) Of Engagement Activity 2021
URL https://www.european-mrs.com/meetings/2021-spring-meeting-0
 
Description Electronmicroscopy Symposium 
Form Of Engagement Activity Participation in an activity, workshop or similar
Part Of Official Scheme? No
Geographic Reach National
Primary Audience Professional Practitioners
Results and Impact Planned symposium to promote the Electron microscope facility. A successful event promoting national engagement to UKRI funded facilities. Advertised internally and through ScotChem and SUPA
Year(s) Of Engagement Activity 2020
URL https://jtsigroup.wp.st-andrews.ac.uk/electron_microscope_facility/
 
Description EnergyCeram 
Form Of Engagement Activity A talk or presentation
Part Of Official Scheme? No
Geographic Reach International
Primary Audience Postgraduate students
Results and Impact European School on Ceramics for Energy Conversion and Storage (EnergyCeram)
The online school aims at presenting a current overview of ceramic materials and technologies for selected energy applications. A topical focus is put on high-temperature power generation (gas turbines, concentrated solar power) and electrochemical applications based on ionic transport (solid oxide fuel cells, gas separation membranes, electrochemical storage).
After a brief introduction of each application field including targets for properties, the relevant ceramic materials will be reviewed and evaluated. In order to be integrated in real devices, they need to fulfil numerous, often contradictory conditions, such as highest ionic and/ or electronic conductivity, stability during operation, processability, etc.

The used online platform will allow for personal interactions (including video chat and screen sharing). Enough breaks are foreseen to stimulate exchanges, offering the opportunity to chat with other participants and meet new people face-to-face or in small groups!
Year(s) Of Engagement Activity 2020
URL https://congress.dkg.de/event/eu_spring_school_001/
 
Description ICTN-KLC, India 
Form Of Engagement Activity A talk or presentation
Part Of Official Scheme? No
Geographic Reach International
Primary Audience Professional Practitioners
Results and Impact International Conference on Thin Films & Nanotechnology: Knowledge, Leadership, & Commercialization

The ICTN-KLC: 2021, the first one of its kind, aims to bring together students, academicians, scientists, technologists, and entrepreneurs working on development and applications of thin films and nanomaterials from lab to commercial (industrial) scale. The inaugural 3-days conference will be organized virtually from the foundation day of the Thin Film Lab (TFL). In addition to scientific talks, there will be sessions dedicated to research ethics, leadership, and entrepreneurship targeted mainly for early career researchers. The conference will consist of plenary/invited talks and contributed papers on various focus areas in Thin Films & Nanotechnology.
Year(s) Of Engagement Activity 2021
URL http://www.ictn-klc.org/
 
Description IVWFC 2021, Italy 
Form Of Engagement Activity A talk or presentation
Part Of Official Scheme? No
Geographic Reach International
Primary Audience Professional Practitioners
Results and Impact Virtual Workshop on Fuel cells - Oral contributions in the different fields of fuel cells/ electrolysers science and technology. Delivered by national and international specialists.
Year(s) Of Engagement Activity 2021
URL https://ivwfc.mater.unimib.it/
 
Description Invited Talk 
Form Of Engagement Activity A talk or presentation
Part Of Official Scheme? No
Geographic Reach International
Primary Audience Professional Practitioners
Results and Impact The greatest challenge facing Solid oxide cells (SOC), in both fuel and electrolysis cell modes (i.e SOFCs and SOECs) is to deliver high, long-lasting electrocatalytic activity while ensuring cost and time-efficient electrode manufacture. Ultimately, this can best be achieved by growing appropriate nanoarchitectures under operationally relevant conditions, rather than through intricate ex situ procedures.

In our approach, metal particles are grown directly from the oxide support though in situ redox exsolution. We demonstrated that by understanding and manipulating the surface chemistry of an oxide support with adequately designed bulk (non)stoichiometry, one can control the size, distribution and surface coverage of produced particles. We also revealed that the emergent particles are generally epitaxially socketed in the parent perovskite which appears to be the underlying origin of their remarkable stability, including unique resistance of metal particles to agglomeration and to hydrocarbon coking, whilst retaining catalytic activit.

Operando redox treatments yield emergent nanomaterials at potentials in excess of 2V. Here we apply this technique to drive steam, CO2 and coelectrolysis processes at emergent metals and alloy particles.
Year(s) Of Engagement Activity 2020
URL https://ecs.confex.com/ecs/prime2020/meetingapp.cgi/Paper/143913
 
Description MEMP 2021 
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 Centre for Materials for Electronics Technology (C-MET), Pune is organizing an International Conference on Multifunctional Electronic Materials & Processing (MEMP 2021) at Pune, India during 8-10 March 2021.
MEMP-2021 provide an opportunity to scientists, researchers, academicians and young students to interact with eminent scientists/technologists working in the field of multifunctional electronic materials for various applications & their processing for making devices.
Materials required for energy storage, energy generation, Nanostructured materials, Quantum dots, Sensors, Neutrino Energy Conversion /storage. Flexible devices, Photonic devices and processing techniques like Additive Manufacturing (3D printing) will be discussed here.
MEMP 2021 will serve as a common platform for discussing the new ideas developments/ breakthroughs and future prospects pertaining to multifunctional electronic materials with some of the leading scientists/ technologists as well as to be acquainted with their experience and knowledge.
Year(s) Of Engagement Activity 2021
URL https://journalsofindia.com/multifunctional-electronic-materials-processing-memp-2021/
 
Description MMC2019 - Dr Aaron Naden 
Form Of Engagement Activity A talk or presentation
Part Of Official Scheme? No
Geographic Reach International
Primary Audience Professional Practitioners
Results and Impact Dissemination of original research at an international conference.
Year(s) Of Engagement Activity 2019
URL https://www.rms.org.uk/discover-engage/event-calendar/mmc2019-microscience-microscopy-congress-2019....
 
Description STACEES Network Launch 
Form Of Engagement Activity A talk or presentation
Part Of Official Scheme? No
Geographic Reach Local
Primary Audience Supporters
Results and Impact The launch of The St Andrews Network for Climate, Energy, Environment and Sustainability (STACEES) is an interdisciplinary research-focused initiative launched in April 2021 at The University of St Andrews.

STACEES' objective is to drive cohesion and capacity in environmental sustainability research at St Andrews, boosting its impact and visibility. The network's vision is to build ambitious, lasting research capabilities that position the University at the centre of international conversations on climate change, energy research and environmental sustainability.
Year(s) Of Engagement Activity 2021
URL https://events.st-andrews.ac.uk/events/sta-cees-network-launch-with-guest-speaker-prof-john-irvine/
 
Description UKRI at COP26 
Form Of Engagement Activity A formal working group, expert panel or dialogue
Part Of Official Scheme? No
Geographic Reach International
Primary Audience Policymakers/politicians
Results and Impact Our role in supporting a Year of Climate Action.

The UN Climate Change Conference (COP26) is underway. We are supporting activities and events that inspire and engage people and promote positive climate action. Whether you are at COP26 or not, register to access our events, exhibitor booths and engage with researchers and innovators.

On these pages you will find out more about:

the role research and innovation play in tackling climate change
events that UK Research and Innovation is hosting and promoting for COP26, and how to sign up and attend
how to join the climate conversation and share your work and ideas.
Year(s) Of Engagement Activity 2021
URL https://www.ukri.org/our-work/responding-to-climate-change/ukri-towards-cop26/