3D Volume Microscopy and TEM Sample Preparation of Complex Hybrid Nanostructures
Lead Research Organisation:
University of Leeds
Department Name: Chemical and Process Engineering
Abstract
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.
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.
Publications
Alotaibi KM
(2017)
Iron supported on bioinspired green silica for water remediation.
in Chemical science
Besselink R
(2020)
Mechanism of Saponite Crystallization from a Rapidly Formed Amorphous Intermediate
in Crystal Growth & Design
Chimupala Y
(2018)
Hydrothermal Synthesis and Phase Formation Mechanism of TiO<sub>2</sub>(B) Nanorods via Alkali Metal Titanate Phase Transformation
in Solid State Phenomena
Cottom J
(2017)
Fabrication and Characterisation of an Adaptable Plasmonic Nanorod Array for Solar Energy Conversion
in Journal of Physics: Conference Series
Cottom J
(2018)
Systematic Analysis of the Coupling Effects within Supported Plasmonic Nanorod Antenna Arrays
in The Journal of Physical Chemistry C
Evans SJ
(2019)
In vitro detection of in vitro secondary mechanisms of genotoxicity induced by engineered nanomaterials.
in Particle and fibre toxicology
Freeman HM
(2019)
Beam-induced oxidation of mixed-valent Fe (oxyhydr)oxides (green rust) monitored by STEM-EELS.
in Micron (Oxford, England : 1993)
H Perez JP
(2020)
Direct Visualization of Arsenic Binding on Green Rust Sulfate.
in Environmental science & technology
Heath GR
(2018)
Visualization of diffusion limited antimicrobial peptide attack on supported lipid membranes.
in Soft matter
Hillier S
(2018)
Correlations among the mineralogical and physical properties of halloysite nanotubes (HNTs)
in Clay Minerals
Hövelmann J
(2019)
Struvite Crystallisation and the Effect of Co2+ Ions
in Minerals
Ilett M
(2020)
Analysis of complex, beam-sensitive materials by transmission electron microscopy and associated techniques.
in Philosophical transactions. Series A, Mathematical, physical, and engineering sciences
Ilett M
(2020)
Application of automated electron microscopy imaging and machine learning to characterise and quantify nanoparticle dispersion in aqueous media.
in Journal of microscopy
Ilett M
(2017)
Cryo-STEM-EDX spectroscopy for the characterisation of nanoparticles in cell culture media
in Journal of Physics: Conference Series
Ilett M
(2023)
In situ electron microscopy techniques for nanoparticle dispersion analysis of commercial sunscreen
in Journal of Nanoparticle Research
Ilett M
(2019)
Cryo-analytical STEM of frozen, aqueous dispersions of nanoparticles.
in Micron (Oxford, England : 1993)
Inam A
(2017)
A high-resolution study of graphite nodule formation in experimental medium-carbon machining steel
in Materials Characterization
Lanigan J
(2017)
Understanding the wear behaviour of non-doped and Si,O-doped diamond-like carbon films
in RSC Advances
Parlett C
(2015)
Spatially orthogonal chemical functionalization of a hierarchical pore network for catalytic cascade reactions
in Nature Materials
Roach L
(2018)
Morphological control of seedlessly-synthesized gold nanorods using binary surfactants.
in Nanotechnology
Roach L
(2022)
Controlling the Optical Properties of Gold Nanorods in One-Pot Syntheses.
in The journal of physical chemistry. C, Nanomaterials and interfaces
Roach L
(2021)
Evaluating Phospholipid-Functionalized Gold Nanorods for In Vivo Applications.
in Small (Weinheim an der Bergstrasse, Germany)
S'ari M
(2018)
Toward Developing a Predictive Approach To Assess Electron Beam Instability during Transmission Electron Microscopy of Drug Molecules.
in Molecular pharmaceutics
Soltanahmadi S
(2019)
Surface Fatigue Behavior of a WC/aC:H Thin-Film and the Tribochemical Impact of Zinc Dialkyldithiophosphate.
in ACS applied materials & interfaces
Stawski T
(2019)
Particle-Mediated Nucleation Pathways Are Imprinted in the Internal Structure of Calcium Sulfate Single Crystals
in Crystal Growth & Design
Stock S
(2021)
The quantitative impact of fluid vs. solid interfaces on the catalytic performance of pickering emulsions.
in Physical chemistry chemical physics : PCCP
Thomas A
(2020)
Effects of metal cation substitution on hexavalent chromium reduction by green rust
in Geochemical Transactions
| 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). Have extended the instrument with cryogrippers for TEM sample liftout using EPSRC grant EP/T024488/1. |
| 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. We have also been awarded additional funds to purchase cryo-grippers so as to allow in-situ liftout of frozen TEM lamella - which we have successfully demonstrated and is a UK first. Since installation we have provided access to a wide range of internal and external users for 3D imaging and preparation of TEM specimens and the examination of cryogenically frozen soft matter specimens. The instrument has been very heavily used in the last 3 years and is now capable of unattended overnight operation. |
| First Year Of Impact | 2017 |
| Sector | Aerospace, Defence and Marine,Agriculture, Food and Drink,Chemicals,Construction,Digital/Communication/Information Technologies (including Software),Electronics,Energy,Environment,Healthcare,Manufacturing, including Industrial Biotechology,Pharmaceuticals and Medical Biotechnology |
| Impact Types | Societal,Economic |
| Description | 3D Nanoscale chemical analysis: a FIBSEM-SIMS facility optimised for soft and composite materials |
| Amount | £1,726,123 (GBP) |
| Funding ID | EP/V028855/1 |
| Organisation | Engineering and Physical Sciences Research Council (EPSRC) |
| Sector | Public |
| Country | United Kingdom |
| Start | 07/2021 |
| End | 06/2025 |
| Description | Bridging the gap between cell and structural biology at the University of Leeds |
| Amount | £418,467 (GBP) |
| Funding ID | 208395/Z/17/Z |
| Organisation | Wellcome Trust |
| Sector | Charity/Non Profit |
| Country | United Kingdom |
| Start | 02/2018 |
| End | 02/2023 |
| Description | Core Equipment at the University of Leeds |
| Amount | £549,999 (GBP) |
| Funding ID | EP/T024488/1 |
| Organisation | Engineering and Physical Sciences Research Council (EPSRC) |
| Sector | Public |
| Country | United Kingdom |
| Start | 02/2020 |
| End | 08/2021 |
| Description | Cryogenic electron microscopy for native state analysis of nanoparticles in liquids |
| Amount | £196,879 (GBP) |
| Funding ID | EP/R043388/1 |
| Organisation | Engineering and Physical Sciences Research Council (EPSRC) |
| Sector | Public |
| Country | United Kingdom |
| Start | 09/2018 |
| End | 02/2021 |
| Description | Crystallisation in the Real World: Delivering Control through Theory and Experiment |
| Amount | £5,436,236 (GBP) |
| Funding ID | EP/R018820/1 |
| Organisation | Engineering and Physical Sciences Research Council (EPSRC) |
| Sector | Public |
| Country | United Kingdom |
| Start | 03/2018 |
| End | 02/2023 |
| 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 | The Leeds EPSRC Nanoscience and Nanoequipment User Facility |
| Amount | £201,946 (GBP) |
| Funding ID | EP/R02863X/1 |
| Organisation | Engineering and Physical Sciences Research Council (EPSRC) |
| Sector | Public |
| Country | United Kingdom |
| Start | 06/2018 |
| End | 11/2020 |
| 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 | 2008,2009,2010,2011,2012,2013,2014,2015,2016,2017,2018,2019,2020,2021 |
| 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, 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 | 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 | 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 |
| Description | Scientific Organisation of Microscience Microscience Microscopy Congresses MMC2013, 2015, 2017, 2019, 2021 |
| 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 | Attendance and presentation at conferences |
| Year(s) Of Engagement Activity | 2013,2015,2017,2019,2021 |
| URL | https://www.mmc-series.org.uk/ |