3D Nanoscale chemical analysis: a FIBSEM-SIMS facility optimised for soft and composite materials
Lead Research Organisation:
University of Leeds
Department Name: Chemical and Process Engineering
Abstract
The increasing complexity of materials that underpin advances in the digital technologies, additive manufacturing, healthcare, food, energy, environmental and fine chemical sectors requires a step-change in semi-quantitative, isotopic and trace chemical analysis from nanoscale volumes, contextualised in their native 3D structure. Furthermore, with urgent societal pressures for sustainable NetZero technologies, rapid analysis of both synthetic and natural materials over multiple length scales, can facilitate their improvement and optimal utilisation. An integrated UHV FIBSEM-ToFSIMS instrument provides an important tool for surface chemical analysis with isotopic and trace element sensitivity and also enables 3D nanoscale chemical characterisation of materials over volumes of 100,000 cubic micrometres via serial ion beam sectioning. This analysis fills a pivotal gap within correlative workflows for the combined structural and chemical imaging of materials at different length scales: between that probed by light and X-rays, and that obtained using analytical transmission electron microscopy, and ultimately atom probe tomography. The new equipment will possess flexibility to study both hard and also soft materials, via the cryo-workflow, thus increasing UK expertise in analysis of important, hybrid organic-inorganic materials. Such a capability opens up new horizons for the characterisation of complex soft solids (and potentially solid/liquid dispersions) used in a wide range of medical, chemical, structural and electronic applications.
Publications
Basaran R
(2024)
Probing the pH-dependency of DC-SIGN/R multivalent lectin-glycan interactions using polyvalent glycan-gold nanoparticles.
in Nanoscale advances
Galloway JM
(2023)
Electron transparent nanotubes reveal crystallization pathways in confinement.
in Chemical science
Gray-Wannell N
(2023)
Morphological features of halloysite nanotubes as revealed by various microscopies
in Clay Minerals
Ilett M
(2023)
In situ electron microscopy techniques for nanoparticle dispersion analysis of commercial sunscreen
in Journal of Nanoparticle Research
Sun C
(2024)
Modulating proton conductivity through crystal structure tuning in arenedisulfonate coordination polymers
in Journal of Materials Chemistry A
| Description | Improved production of cross-sectional and 3D volume microscopy of soft materials systems |
| Exploitation Route | External user access schemes via Royce Institute and also Case Studies |
| Sectors | Agriculture Food and Drink Chemicals Energy Environment Healthcare Manufacturing including Industrial Biotechology Pharmaceuticals and Medical Biotechnology |
| Description | Analytical electron and ion beam microscopy to enable precision engineering of complex chemical products for high value technology sectors |
| Amount | £1,500,000 (GBP) |
| Funding ID | EP/X040992/1 |
| Organisation | Engineering and Physical Sciences Research Council (EPSRC) |
| Sector | Public |
| Country | United Kingdom |
| Start | 03/2024 |
| End | 02/2028 |
| Title | Cryo-liftout of TEM lamella using cryogrippers |
| Description | Using cryo-cooled mechanical grippers we have successfully developed a protocol for performing in-situ liftout of cryogenically coolled TEM lamella thinned by the ion beam milling in a dual beam FIBSEM. This is highly important for the study of soft matter microstructures in their native state, We offer this capability to both internal and external users |
| Type Of Material | Improvements to research infrastructure |
| Year Produced | 2023 |
| Provided To Others? | No |
| Impact | Extended abaility to look at beam sensitive and vacuum sensitive materials in their native state, |
| Description | Quorum Cryo-liftout |
| Organisation | Quorum Review- Independent Review Board |
| Country | United States |
| Sector | Private |
| PI Contribution | Collaboration with company Quorum on in-situ liftout of frozen TEM samples |
| Collaborator Contribution | Collaboration with company Quorum on in-situ liftout of frozen TEM samples |
| Impact | none so far |
| Start Year | 2017 |
| Description | Tescan |
| Organisation | TESCAN Brno s.r.o. |
| Country | Czech Republic |
| Sector | Private |
| PI Contribution | As part of the equipment tender process initiated discussions about becoming a beta test site for the development of a new transmission electron microscope |
| Collaborator Contribution | Potential provision of a new beta transmission electron microscope plus research collaboration. Full agreement yet to be reached. |
| Impact | Still under discussion |
| Start Year | 2021 |
| Description | Thermo Fisher |
| Organisation | Thermo Fisher Scientific |
| Country | United States |
| Sector | Private |
| PI Contribution | As part of the equipment tender process initiated discussions about provision of a new workhorse transmission electron microscope (TEM) and also discussing the potential for becoming a project partner on a bid for a new advanced scanning TEM |
| Collaborator Contribution | Provision of a new workhorse TEM and potentially access to new R&D for a grant proposal for a new advanced TEM |
| Impact | None as yet |
| Start Year | 2021 |
| Description | Annual Royal Microscopical Society School in Elecron Microscopy - every Spring or Summer 2008 onwards |
| 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 | Week long Training School for users of the technique |
| Year(s) Of Engagement Activity | 2008,2009,2010,2011,2012,2013,2014,2015,2016,2017,2018,2019,2020,2021 |
| Description | Be Curious Science Outreach event |
| Form Of Engagement Activity | Participation in an open day or visit at my research institution |
| Part Of Official Scheme? | No |
| Geographic Reach | Regional |
| Primary Audience | Schools |
| Results and Impact | Microscopy Demonstrations |
| Year(s) Of Engagement Activity | 2022 |
| URL | https://www.leeds.ac.uk/news-university/news/article/5058/explore-learn-and-create-at-be-curious-202... |
| Description | Be Curious Science Outreach event |
| Form Of Engagement Activity | Participation in an open day or visit at my research institution |
| Part Of Official Scheme? | No |
| Geographic Reach | Regional |
| Primary Audience | Schools |
| Results and Impact | Microscopy Talk, Activities and Display at Be Curious Festival at University of Leeds, Annual event every March |
| Year(s) Of Engagement Activity | 2016,2017,2018,2019,2020 |
| URL | http://www.leeds.ac.uk/info/4000/around_campus/460/be_curious_festival-about_leeds_and_yorkshire |
| Description | Be Curious Scientific Outreach event |
| Form Of Engagement Activity | Participation in an open day or visit at my research institution |
| Part Of Official Scheme? | No |
| Geographic Reach | Regional |
| Primary Audience | Public/other audiences |
| Results and Impact | Microscopy Demonstrations |
| Year(s) Of Engagement Activity | 2023 |
| URL | https://www.leeds.ac.uk/news-university/news/article/5287/inspire-create-and-explore-at-be-curious-2... |
| Description | Co-organisation of Royal Society Discussion Meeting, Dynamic in-situ microscopy relating structure and function |
| 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 | Fast-track discussion meeting organised by Dame Pratibha Gai FREng FRS, Professor Edward Boyes, Professor Rik Brydson and Professor Richard Catlow FRS. October 21-22 2019 This meeting evidenced and advanced development in dynamic in-situ environmental electron, scanning probe, optical and fast time resolved microscopy and computer modelling studies of vital interest in the chemical, physical and life sciences, underpinning technologies of high commercial and societal value. It focused on the pivotal role of imaging and spectroscopy for dynamic processes across the sciences to access previously invisible aspects of real world processes. An accompanying journal issue for this meeting was published in Philosophical Transactions of the Royal Society A. |
| Year(s) Of Engagement Activity | 2019 |
| URL | https://royalsociety.org/science-events-and-lectures/2019/10/in-situ-microscopy/ |
| Description | Presentation at Industry Day |
| Form Of Engagement Activity | A talk or presentation |
| Part Of Official Scheme? | No |
| Geographic Reach | International |
| Primary Audience | Industry/Business |
| Results and Impact | Presentation of the Programme Grant activity to members of the Industry Club (20 members) of the Institute of Process Research and Development at Weetwood Hall, Leeds |
| Year(s) Of Engagement Activity | 2022 |
| Description | Royce Institute Workshop for PhD students |
| 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 | A three day residential workshop for 15-20 PhD students, particularly targeted at those in CDTs, to showcase (mostly) Royce facilities at Leeds. Basic structure was lectures then demonstrations. |
| Year(s) Of Engagement Activity | 2020 |