A Facility for Cryo-Enabled Multi-microscopy for Nanoscale Analysis in the Engineering and Physical Sciences (Cryo-EPS)

Lead Research Organisation: Imperial College London
Department Name: Materials

Abstract

We are facing unprecedented global challenges around climate change, clean energy, water and sustainability - and these have, at their core, materials solutions. Critical materials for future technologies are often highly complex on multiple length scales, and hence extremely difficult to characterise with a single technique. They commonly involve low atomic weight, mobile elements (e.g. hydrogen, lithium, carbon, sulfur) that are the most challenging to quantitatively characterise in their in-operando state, due to their high rates of diffusion, reactivity and often very low contrast by conventional imaging techniques.
Examples of such materials systems include; materials for hydrogen production and storage, battery systems; catalysts to generate new fuels or facilitate decarbonation of industrial processes; interfaces between soft- and hard-matter relevant to hybrid electronics and 'soft' robotics; as well as liquids or liquid- solid interfaces that are critical across the whole engineering and physical sciences research space from geological carbon sequestration, to lubrication in engines, to chemistry and bioengineering.

We will create a world-leading cryo-EPS facility to act as a collaborative hub for research that will underpin the UK ambition for a net zero carbon future and a more sustainable society. It will enable the quantitative atomic to micro-scale investigation of light elements that are critical to a host of new technologies associated with a transition to a sustainable, resilient and healthy future society, providing new scientific insights that will drive technological innovation.

The equipment will enable the quantitative investigation of light elements across orders of magnitude in length scale - from the micron to the atomic scale, providing an unprecedented opportunity for a step change in our fundamental understanding of these materials structure and chemistry - and ultimately their behaviour
This facility will be based around a cryo hub that will allow samples to be transferred under high vacuum and at cryo conditions between three instruments (i) an atom probe, uniquely positioned to quantitively measure chemical composition of light mobile elements; (ii) a transmission electron microscope with a vacuum-cryo holder and optimised to measure the structure of sensitive samples and also their local bonding environment; (iii) a plasma FIB to allow samples to be prepared for both the atom probe and TEM which have both low contamination and also little damage, and able to perform large-scale 3D imaging.
The combination of these instruments will give the UK a powerful characterisation capability that is unique worldwide, putting UK scientists in a leading position to tackle important and urgent global challenges.

Publications

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Birch RM (2023) A Conventional and High Resolution Electron Backscatter Diffraction (EBSD) Study of Stress Fields around Hydrides in Zircaloy-4. in Microscopy and microanalysis : the official journal of Microscopy Society of America, Microbeam Analysis Society, Microscopical Society of Canada

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El-Zoka A (2023) The Fate of Water in Hydrogen-Based Iron Oxide Reduction in Advanced Science

 
Description A key part of this project relies on the ability to produce high quality samples under a complete cryo work flow. In the past his has been achieved for TEM samples, however, here we show that this can also be achieved for atom probe samples.

This has now been extend to full cryo work flow where samples are made from a frozen liquid and transferred under cryo conditions to the atom probe to allow visualisation of chemical species in the liquid but close to the interface. This was a goal of this project at the outset.

This opens up the possibility to study the chemistry of a range of frozen liquids, particularly where it is close to solid interface such in a electro chemical system such as a battery or an area of corrosion.
Exploitation Route There is interest in this from number of commercial companies.
Sectors Aerospace

Defence and Marine

Energy

Transport

 
Description Organising the workshop in 4D-STEM for postgraduate researchers
Geographic Reach Local/Municipal/Regional 
Policy Influence Type Influenced training of practitioners or researchers
Impact The workshop has not happened yet. But we hope this will provide students with the skills to process microscopy data using open source coding methods.
 
Description Postgraduate Electron Microscopy Lecture Course
Geographic Reach Local/Municipal/Regional 
Policy Influence Type Influenced training of practitioners or researchers
 
Description Practical training of users on Electron Microscopy equipment
Geographic Reach Local/Municipal/Regional 
Policy Influence Type Influenced training of practitioners or researchers
 
Description Corrosion at the Atomic Scale (CAtS)
Amount £70,000 (GBP)
Organisation The Royal Society 
Sector Charity/Non Profit
Country United Kingdom
Start 03/2023 
End 08/2024
 
Description High Voltage Ceramic Heating (ETC-2022-5818)
Amount £477,000 (GBP)
Organisation Shell Global Solutions International BV 
Sector Private
Country Netherlands
Start 01/2023 
End 01/2025
 
Description INFUSE: Interface with the Future - Underpinning Science to Support the Energy transition
Amount £4,191,429 (GBP)
Funding ID EP/V038044/1 
Organisation Engineering and Physical Sciences Research Council (EPSRC) 
Sector Public
Country United Kingdom
Start 08/2021 
End 08/2026
 
Description Research Fellows Enhanced Research Grant
Amount £170,000 (GBP)
Funding ID RF\ERE\210200 
Organisation The Royal Society 
Sector Charity/Non Profit
Country United Kingdom
Start 01/2022 
End 03/2023
 
Description Research Fellows Enhanced Research Grant
Amount £270,000 (GBP)
Organisation The Royal Society 
Sector Charity/Non Profit
Country United Kingdom
Start 03/2023 
End 12/2025
 
Description Atom Probe Tomography of High Entropy Alloys 
Organisation Korea University
Country Korea, Republic of 
Sector Academic/University 
PI Contribution We have analyzed the atomic scale chemistry of Co-Ni-Mo-Al alloys using atom probe tomography. We have also analysed hydrogen absopriton inside iron nitrides susccessfully
Collaborator Contribution Our partner have fabricated and processed the samples.
Impact This is a collaboration involving the areas of hydrogen materials, high entropy alloys and atom probe tomography.
Start Year 2024
 
Description Cryo-APT of Enclosed Liquids in 3D Printed Structures 
Organisation Max Planck Society
Department Max Planck Institute for Iron Research
Country Germany 
Sector Charity/Non Profit 
PI Contribution Our collaborator in Germany have been 3D printing Cu-based structures with the capability to trap limited volumes of liquid within. We have been able to perform cryogenic scanning electron microscopy and cryogenic atom probe tomography showing the liquid-solid interface between the 3D printed Cu and enclosed liquids for the first time.
Collaborator Contribution Our partner has been able to systematically modify their technique of 3D printing to make structures with dimensions that are more suitable for cryo-APT analysis.
Impact This is a multi-disciplinary collaboration involving the areas of 3D printed microstructures, cryogenic atom probe tomography and electrochemistry.
Start Year 2023
 
Description Nanoscale investigation of interfaces in ceramic composites 
Organisation Rolls Royce Group Plc
Country United Kingdom 
Sector Private 
PI Contribution We started a feasibility study to understand how diffusion happens in different interfaces found in ceramic composites. This included interfaces between dissimilar materials (BN - SiC) and interfaces in similar materials (different grain boundaries in SiC). We used Atom Probe Tomography (APT) to show feasibility to observe and quantify diffusion in different interfaces and correlate it the microstructure defined with TEM images.
Collaborator Contribution The partners provided: a range of ceramic composite samples with complex microstructures, funding for PDRA time and attendance to meetings to discuss the data.
Impact The outcome of this work was a feasibility study to show which interfaces which can explore. We concluded that interfaces in polycrystalline materials are easier to characterise while interfaces in dissimilar materials are more challenging and require further work.
Start Year 2022
 
Description Chair Session at the 244th Electrochemical Society Meeting 
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 Chairing a session on electrodeposition into complex geometries at the 244th ECS Meeting in Sweden, 2023.
Year(s) Of Engagement Activity 2023
 
Description Cryo-EM Facility - Opening 
Form Of Engagement Activity Participation in an open day or visit at my research institution
Part Of Official Scheme? No
Geographic Reach International
Primary Audience Other audiences
Results and Impact Around 60 people attended the opening of the new Cryo-EM Facility, many of whom were alumni of the department working in Industry or Education. This event provided a platform to show off our new facility, discuss current and future research, and form collaborations.
Year(s) Of Engagement Activity 2023
 
Description Imperial Lates: Tiny Science 
Form Of Engagement Activity Participation in an open day or visit at my research institution
Part Of Official Scheme? No
Geographic Reach National
Primary Audience Public/other audiences
Results and Impact Imperial Lates is a themed outreach evening open to the general public where Imperial College London researchers can present and discuss their research. The theme of the November Lates was Tiny Science. Members of the NAME programme grant and Cryo EPS discussed the use of ion implantation in maser research through the use of a large scale "ion smash" game which demonstrated the principles and applications of the P-NAME ion implantation tool and the why we need cryogenic atomic scale microscopy to analyse these single ion implantation centres.
Year(s) Of Engagement Activity 2022
URL https://www.imperial.ac.uk/events/152709/imperial-lates-tiny-science/
 
Description Interview for DW International 
Form Of Engagement Activity A press release, press conference or response to a media enquiry/interview
Part Of Official Scheme? No
Geographic Reach International
Primary Audience Media (as a channel to the public)
Results and Impact An interview on green steel and related research.
Year(s) Of Engagement Activity 2023
 
Description MRS Fall 2022 meeting symposium organisation and chairing: Higher-Order Topological Structures in Real Space-From Charge to Spin 
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 The increasingly cross-disciplinary worldwide activity in materials research manifests itself every year in the MRS Fall Meetings. Featuring over 50 symposia and attended by as many as 6,000 researchers from every corner of the globe, the annual Fall Meeting in Boston's Hynes Convention Center and Sheraton Boston Hotel is the preeminent annual event for those in the field of materials research. This symposium aims to bring together scientific experts and young scientists with an interest in topologically non-trivial charge and spin textures that arise in real space, fostering interactions and advancing knowledge of higher-order topological structures in ferroelectrics, multiferroics and magnetic materials.
Year(s) Of Engagement Activity 2022
URL https://www.mrs.org/meetings-events/fall-meetings-exhibits/2022-mrs-fall-meeting/symposium-sessions/...
 
Description MRS Fall 2023 meeting symposium organisation and chairing: Higher-Order Topological Structures in Real Space-From Charge to Spin 
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 The increasingly cross-disciplinary worldwide activity in materials research manifests itself every year in the MRS Fall Meetings. Featuring over 50 symposia and attended by as many as 6,000 researchers from every corner of the globe, the annual Fall Meeting in Boston's Hynes Convention Center and Sheraton Boston Hotel is the preeminent annual event for those in the field of materials research.
This symposium aims to bring together scientific experts and young scientists with an interest in topologically non-trivial charge and spin textures that arise in real space, fostering interactions and advancing knowledge of higher-order topological structures in ferroelectrics, multiferroics and magnetic materials.
Year(s) Of Engagement Activity 2023
URL https://www.mrs.org/meetings-events/fall-meetings-exhibits/2023-mrs-fall-meeting/call-for-papers/det...
 
Description MRS Spring 2023 Cryogenic TEM and APT symposium organisation and Chairing 
Form Of Engagement Activity Participation in an activity, workshop or similar
Part Of Official Scheme? No
Geographic Reach International
Primary Audience Postgraduate students
Results and Impact Organised and Chairing the MRS Spring 2023 symposium: Advances in Cryogenic Transmission Electron Microscopy and Spectroscopy for Quantum and Energy Materials
Year(s) Of Engagement Activity 2023
URL https://www.mrs.org/meetings-events/spring-meetings-exhibits/2023-mrs-spring-meeting/call-for-papers...
 
Description Neil Alford - Presentation and lab tour of NAME and Royce to CNRS delegation 
Form Of Engagement Activity A formal working group, expert panel or dialogue
Part Of Official Scheme? No
Geographic Reach International
Primary Audience Third sector organisations
Results and Impact Presentation to a delegation from CNRS
Year(s) Of Engagement Activity 2023
 
Description Organisation and chairing of EMAG symposia at Microscience Microscopy Congress 2023 
Form Of Engagement Activity Participation in an activity, workshop or similar
Part Of Official Scheme? No
Geographic Reach International
Primary Audience Postgraduate students
Results and Impact MMC 2023 brought together around 2000 people from across the microscopy world and related industries. Speakers from across the UK and the world were invited to present their latest research. Discussion in symposia as well as informal settings resulted in interest and collaborations which could only be carried out using the unique capabilities of the Cryo-EM facilities equipment.
Year(s) Of Engagement Activity 2023
URL https://www.mmc-series.org.uk/
 
Description Organisation and chairing of Institute of Physics EMAG 2022 Conference at Imperial College London 
Form Of Engagement Activity Participation in an activity, workshop or similar
Part Of Official Scheme? No
Geographic Reach National
Primary Audience Other audiences
Results and Impact Around 130 scientists and industry partners in the area of transmission electron microscopy came together to discuss research and developments in the area of electron microscopy. Awareness of the Cryo Electron Microscopy facility was made through scientific presentations, informal discussions and tours of the new facility
Year(s) Of Engagement Activity 2022
URL https://iop.eventsair.com/emag2022/
 
Description Organiser and chair of RMS EM-UKI 2024 Symposium 
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 Around 100 research Technical Professionals and academic staff me to discuss the developments, challenges and research being carried out in facilities such as ours, around the country. Expert knowledge was shared through talks, group discussions and informal meetings. There were specific discussions relating to how our facility was run, best practice from other facilities, and several inquiries about collaborating on projects using our equipment
Year(s) Of Engagement Activity 2024
URL https://www.rms.org.uk/rms-event-calendar/2024-events/em-uki.html
 
Description Roadmap for Electron Microscopy in the Physical Sciences - Working Group 
Form Of Engagement Activity A formal working group, expert panel or dialogue
Part Of Official Scheme? No
Geographic Reach National
Primary Audience Professional Practitioners
Results and Impact Participation in the 'Coordination of Training and Staff Development' working group, part of a national project to refresh the Roadmap for Electron Microscopy in the Physical Sciences. Responses were collated from Lab leader and user surveys from the UK resulting in the formation of working groups which will give recommendations for the roadmap.
Year(s) Of Engagement Activity 2023,2024
 
Description School Visit for International Women's day (Tower Hamlets, London) 
Form Of Engagement Activity A talk or presentation
Part Of Official Scheme? No
Geographic Reach Regional
Primary Audience Schools
Results and Impact About 80 students attended an International Women's day event at their A-Level College. As a scientist I talked about my job and how I got to where I am. This event reached both A-level students and adult learners who were stuyding English as a second language.
Year(s) Of Engagement Activity 2023