3D Volume Microscopy and TEM Sample Preparation of Complex Hybrid Nanostructures

Lead Research Organisation: University of Leeds
Department Name: Chemical and Process Engineering


Use of a focused ion beam (FIB) in a dual beam, analytical scanning electron microscope (SEM) for serial ion beam sectioning of solids allows the investigation of the three dimensional (3D) chemical micro- and nanostructure over volumes of hundreds of cubic microns, so called 3D volume microscopy, at resolutions greater than that achievable using X-ray microtomography. In addition, it is possible to extract site-specific thin transmission electron microscopy (TEM) cross-sections for the higher resolution analysis of surfaces or interfaces within the microstructure. The use of a liquid nitrogen-cooled sample cryo-stage reduces ion beam damage and permits the application to beam-sensitive samples such as hybrid inorganic-organic materials, organics and also frozen samples which is otherwise extremely challenging. Furthermore, the inclusion of a cooled nanomanipulator and a scanning TEM (STEM) detector enables in-situ imaging of frozen TEM lamella that, in principle, could be cryo-transferred to an external cryo-TEM for additional analysis. As well as reducing damage in conventional inorganic materials, such a capability opens up new horizons for the characterisation of complex soft solids (and potentially liquid dispersions) used in a wide range of medical, chemical, structural and electronic applications.

Planned Impact

In terms of economic impact, the University of Leeds has a longstanding track record of translating research to industrial end-users though direct collaboration, licensing of IP, or spin-out, forming a proven model for future translational activity. Many highly successful translational areas are of direct relevance to the potential output of the new cryo-FIBSEM capability, these include sectors such as medical technologies, complex particulate formulated products and ICT. Application in many of these areas will have significant wider societal benefits.
In terms of skills, the new equipment will enhance the skills of a range of postdoctoral researchers and also Ph.D. students in the 8 EPSRC Centres for Doctoral Training (CDTs) associated with Leeds and also those external users from outside Leeds. Additionally there will be impact on the skills of industrial collaborators and also Leeds undergraduates as part of research-led teaching.
We will ensure we communicate the importance and impact of science and engineering enabled by the new equipment to the wider public, policy makers, other funders, charities, governments and political leaders, and demonstrate societal and economic benefits.
Description We have begun to develop methods for 3D volume microscopy using FIB/SEM of cryo samples. We have begun to study a range of materials from polymers, emulsion, biological materials.
Exploitation Route They could gain access to the instrument via our open access user schemes via Royce recurrent funding and also by our new 2 years LENNF user access grant (2018-2020)
Sectors Aerospace, Defence and Marine,Agriculture, Food and Drink,Construction,Energy,Environment,Healthcare,Manufacturing, including Industrial Biotechology,Pharmaceuticals and Medical Biotechnology

URL https://engineering.leeds.ac.uk/info/201503/research_facilities/73/leeds_electron_microscopy_and_spectroscopy_centre/
Description The Dual-beam FEI Helios G4 CX high resolution monochromated Field Emission Gun Scanning Electron Microscope (FEG-SEM) with precise Focused Ion Beam (FIB), a 150mm2 Oxford Instruments X-Max SDD detector, a Quorum cryo-stage and coating/transfer unit and a range of etch and deposition capabilities for Slice & View acquisition of multi signal 3D data sets (3D volume microscopy) and in-situ TEM sample preparation has been installed in easter 2017 and progress has been made with the automated FIB operation, use of the cryo-stage and collection of 3D datasets via study of a range of samples from polymers, emulsions and colloids and biological materials.
First Year Of Impact 2017
Sector Agriculture, Food and Drink,Chemicals,Energy,Environment,Healthcare,Manufacturing, including Industrial Biotechology,Pharmaceuticals and Medical Biotechnology
Impact Types Societal,Economic

Description LENNF Facility
Amount £200,000 (GBP)
Organisation Engineering and Physical Sciences Research Council (EPSRC) 
Sector Public
Country United Kingdom
Start 06/2018 
End 06/2018
Description FEI Titan 
Organisation FEI company
Department FEI United Kingdom
Country United Kingdom 
Sector Private 
PI Contribution Electron Microscopy of Organic Crystals for Pharmaceutical applications - investigation of methodologies for high resolution imaging and analysis
Collaborator Contribution Application of techniques developed for FEI to the study of Pharmaceutical materials
Impact Various conference papers and talks so far. Also has involved PhD studentships and consultancy work with AstraZeneca and Haldor Topsoe, Denmark
Start Year 2016
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 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
Description Attendance at Microscience Microscience Microscopy Congresses MMC2013, 2015 and 2017 
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 Attendance and presentation at conferences
Year(s) Of Engagement Activity 2013,2015,2017
URL https://www.mmc-series.org.uk/
Description BBC Radio 4 interview 
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 Public/other audiences
Results and Impact Interview on Nanogold on BBC Radio 4 Inside Science Broadcast 5 March at 16.30 GMT
Year(s) Of Engagement Activity 2020
URL https://www.bbc.co.uk/programmes/m000fw1n
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, March 2019.
Year(s) Of Engagement Activity 2019
URL http://www.leeds.ac.uk/info/4000/around_campus/460/be_curious_festival-about_leeds_and_yorkshire