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.
 
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 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 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 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