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.
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.
Organisations
- Imperial College London (Lead Research Organisation)
- Korea University (Collaboration)
- Rolls Royce Group Plc (Collaboration)
- Max Planck Society (Collaboration)
- Rosalind Franklin Institute (Project Partner)
- University of Manchester (Project Partner)
- BP (United Kingdom) (Project Partner)
- Ceres Power (United Kingdom) (Project Partner)
- Camfridge (United Kingdom) (Project Partner)
- National Physical Laboratory (Project Partner)
- Rolls-Royce (United Kingdom) (Project Partner)
- Diamond Light Source (Project Partner)
- Cameca (France) (Project Partner)
- University of Oxford (Project Partner)
- Shell (United Kingdom) (Project Partner)
- SKF Group (UK) (Project Partner)
- University of Leeds (Project Partner)
Publications
Yoo S
(2023)
Dopant Evolution in Electrocatalysts after Hydrogen Oxidation Reaction in an Alkaline Environment
in ACS Energy Letters
Woods EV
(2023)
A Versatile and Reproducible Cryo-sample Preparation Methodology for Atom Probe Studies.
in Microscopy and microanalysis : the official journal of Microscopy Society of America, Microbeam Analysis Society, Microscopical Society of Canada
Woods E
(2023)
Scalable substrate development for aqueous sample preparation for atom probe tomography
in Journal of Microscopy
Wang S
(2023)
Near-atomic scale chemical analysis of interfaces in a La(Fe,Mn,Si)13-based magnetocaloric material
in Scripta Materialia
Wang S
(2022)
The effect of hydrogen on the multiscale mechanical behaviour of a La (Fe, Mn, Si) 13-based magnetocaloric material
in Journal of Alloys and Compounds
Wang S
(2024)
Shear and delamination behaviour of basal planes in Zr3AlC2 MAX phase studied by micromechanical testing
in Scripta Materialia
Wang S
(2023)
Determining the fundamental failure modes in Ni-rich lithium ion battery cathodes
in Journal of the European Ceramic Society
Wang D
(2024)
Al-Mn-based decagonal quasicrystal in AZ magnesium alloys and its nucleation on Al8Mn5 during solidification
in Scripta Materialia
Sun J
(2023)
Doping density, not valency, influences catalytic metal-assisted plasma etching of silicon
in Materials Horizons
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 |