High Five: Resolution, Sensitivity, in operando Control, Ultra High Vacuum and Ion Sectioning in a Single Instrument

Lead Research Organisation: Imperial College London
Department Name: Materials


The proposed instrument is a novel combination of ultra-high vacuum (UHV) Plasma Focused Ion Beam SIMS (PFIB-SIMS) that provides a step change in performance of state-of-the-art instrumentation in terms of resolution, sensitivity and applicability. Additional features are dual dynamic positive and negative ion detection, micro-structural analysis, electrical and thermal control for the performance of in operando studies and handling of air-sensitive materials by the incorporation of a pre-chamber. This design, unique worldwide, will enable the chemical quantification of complex surfaces with nanometric resolution and 3D chemical and microstructural reconstruction filling the dimensionality gap in the existing SIMS and FIB technology.
The configuration and components used are at the forefront of materials sectioning and surface characterisation design in a UHV environment. The source of the secondary ions is the gas plasma focused ion beam (FIB) source and column that can produce either oxygen ions or xenon ions with a focus of 25nm for the highest lateral resolutions. This source is also able to section hard and soft materials to length scales of up to a millimetre for sub-surface bulk features by 3D serial-sectioning and characterisation. Low energy surface dosing with caesium is also available for enhancing the secondary ion yields of electronegative elements (e.g. O).
Simultaneous positive and negative SIMS ion detection has been pioneered at Imperial College and is now optimised by ion trajectory modelling in this unique SIMS analysis configuration. Samples with both roughness and form are suitable as low electrical fields are inherent for signal extraction by the two electric quadrupole-based mass spectrometers. Sample cooling and heating is available, also in-situ-electrical contacts for IV testing and grounding at sample surfaces.
Apart from the usual loadlock for a UHV instrument, there will be a second preparation/load-lock chamber for sample processing by temperature control and electrical contacts to mirror the main SIMS analysis chamber facilities. Additionally it will be possible to control the anneal gas ambient to atmospheric pressure with a gas analysis facility. The preparation/load-lock chamber provides a means of transferring air-sensitive samples in vacuum or gas environment from other preparation and characterisation facilities such as a dry Glove-box, SEM, XPS, and Diamond for example. A unique feature of the instrument configuration is the provision for obtaining optical images from samples in both load-locks including optical interference images for topography assessment.
The instrument configuration is designed with inherent future-proofing in mind as both the analysis chamber and the preparation/load-lock have large volumes and spare access ports. In the analysis chamber, the use of a large working distance, ~15mm, low electric field extraction for the SIMS signal and accurate 5-axis stage movements means that there is available solid-angle access to the sample target position within the analysis chamber.
The instrument will be placed in an existing specialist surface analysis laboratory where high performance SIMS/LEIS equipment is located and staffed by permanent ion beam specialists with world leading expertise in optimising ion beam analysis conditions and methodologies. Finally, assistance in data interpretation will be available to the user as well expertise in the operation of High Five.

Planned Impact

The impact of the research enabled by this proposal will be significant and wide ranging due to the breadth of scientific disciplines of the applicants. The impact of the research will be most immediately felt in the areas of physical, chemical, and biological science, along with the engineering and manufacturing disciplines. The realisation of this globally unique analytical instrument, with unprecedented ion beam specifications coupled with in situ sample preparation, and in operando sample analysis will have a dramatic impact in the field of surface analysis. High Five will place UK scientists at the vanguard of this discipline.
During the grant period the main areas of academic impact will be in the areas of research as described in the full case for support. In brief, these areas are: energy conversion and storage, engineering alloys, photonic and electronic materials, medical imaging and biomedical science and engineering. In all of these cases, High Five will enable researchers to ascertain a greater understanding of fundamental ionic process that will improved efficiencies and lifetimes of devices, and better understanding of biological processes that cause a range of debilitating diseases. Importantly, the addition of the High Five instrument in the Materials Department will create a globally important hub of excellence in surface analysis and knowledge transfer. The placement of High Five in the well-established surface analysis lab, with a strong history of training and developing expertise in surface analysis, will draw in the best young researchers at both Post-Doc and PhD level. The multidisciplinary aspect of the instrument and lab will be a unique environment for researchers to develop new collaborations, and realise new correlative methods in materials analysis and characterisation. There will also be a great interest from industrial partners for collaborations, as evidenced by the letters of support.
Aside from the academic impacts of the research there will be many industrial and commercial impacts to be gained from the realisation of High Five. The immediate impact of the successful outcome of the proposal will secure the UK's global position as a world leader in high resolution surface analysis instrumentation. The project will also secure and develop both Hiden Analytical and Oregon Physics international competitiveness, expand their instrument repertoires and develop export markets. This collaboration between scientists and instrument developers clearly highlights the need for the exchange of ideas in the field of surface analysis, and adds to the standing of the proposal.
The most important impact of the outputs of High Five will be upon the society at large. The research described in the full case for support is aimed at improving a wide range of facets of the society in which we live. This includes for example, improving our knowledge and understanding in the area of non-fossil based, environmentally benign energy supplies like fuel cells, batteries and supercaps. This will lead to an improved environment for all, more efficient and innovative use of precious resources.
In the area of healthcare, the planned research will be profound. The work set out in the medical imaging section will aim to optimise therapeutic cancer treatments in order to reduce their unwanted side effects dramatically improving many patient's quality of life. The studies in the biomedical arena aim to investigate the development of AMD, calcification present in atherosclerosis for example, and biological connections between AMD other degenerative diseases such as Alzheimer's. The positive socio-economic impact of the successful implementation of this unique instrument in the domain of healthcare alone will run to many millions, as a better understanding of these debilitating diseases will result in better treatments, patient care and more efficient use of healthcare finances.


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Baiutti F (2021) Direct Measurement of Oxygen Mass Transport at the Nanoscale in Advanced Materials

Description This grant was awarded to develop a new capability unique worldwide. So far we have been able to incorporate two secondary ion mass spectrometers to an Ultra High Vacuum (UHV) chamber and integrate two ante-chambers that will allow introduction of electric contacts, isotopic labelling with gases and add a thermal treatment to the samples (liquid nitrogen-300C). This is a significant technical advance and we have successfully demonstrated the function of the complete system. The plasma ion source has also been incorporated and we have now achieved the specified spot size of 25 nm. A further system upgrade was required which was installed in late 2021 by Oregon Physics, so the system is now as specified. The system is now operational and the first analyses have begun on different set of samples to prove different equipment capabilities. Initial data acquired from the NMC type Li battery electrode has demonstrated that thin surface layers are easily identified using this new instrument, with far superior chemical specificity than is possible with conventional ToF-SIMS. These preliminary results are exciting and promise significant future findings. User training is also underway to ensure rapid acceleration of outputs.
Exploitation Route It is too early to say conclusively, but we expect significant impact of Hi5 once it is fully operational. We have growing interest in different disciplines of materials science to perform experiments. The equipment will be able to reveal chemical aspects of materials and devices in a way never done before in terms of resolution, sensitivity, in situ characterization and ability for 3D chemical and microstructural reconstruction. We expect this to have a great impact in the science that will be delivered and also in the development of surface analysis techniques. There is already significant international interest from partners worldwide, and this equipment will support the objectives of multiple awards, including at least two EU grants and one RAEng Research Chair immediately, with further awards anticipated.
Specific advances made so far are:
1) Introduction of labelled gases:
A reservoir of oxygen-18 gas has been built. This labelled dry gas reservoir will be attached to the separate load-Lock to provide a static labelled gas ambient atmosphere. The oxygen-18 gas is recoverable.
Moist labelled ambient atmospheres with heavy water and oxygen-18 water have required new reservoirs to be built and tested, and this work is complete. These reservoirs can be attached to the load-lock for a labelled moisture content in a static gas ambient within the load-lock.
The 'Hi5' vacuum system has been modified so that the static gas ambient in the load-lock can be sampled and analysed using the residual gas analysis function of the SIMS detectors in the main chamber of 'Hi5'.
2) Electrical probing
Two electrical probes (Kleindiek MM3A micromanipulators) are available to use on samples processed in the load-lock. All the electrical feedthrough connections have been completed and leak tested for operation of the micro-manipulators and the triaxial connectors for low-current, low capacity & resistance loss for electrically probing small features on the sample. During this period we have also integrated the following items:
3) Optical imaging of sample in the vacuum
The provision of reflection microscopy for samples within the vacuum envelope of Hi5 is complete with normal incidence imaging through an optical-quality window and the option of up to 1000X magnification using long-working distance objectives.
Interference microscopy of samples in the vacuum is a work-in-progress.
4) Transfer of air-sensitive from dry box
Sample transfer plans and vacuum transfer suitcase designs were hampered by the in-completeness of the arrangements within the 'Hi5' instrument for sample transfer, cooling and heating. These features represented the last 'snags' of the parts of 'Hi5' designed and built by Hiden Analytical. These issues have now been resolved.
A number of potential designs were considered and discussions had with the those responsible for other vacuum analytical instruments in the Department of Materials (XPS & SEM) in order to achieve compatibility and transferability. A complete vacuum transfer system has now been constructed offering compatibility with multiple platforms in the department.
5) The plasma column ion beam has been incorporated and the focus is on smooth vibrations to achieve nm spot size

The Hi5 is able to undertake simultaneous SE and SI imaging and simultaneous positive and negative ion detection under different currents. We have successfully tested :
- Metal alloys
-Ceramic bulk materials with poly crystalline nature
-Ceramic epitaxial thin films with multilayered structures
Sectors Aerospace, Defence and Marine,Chemicals,Construction,Digital/Communication/Information Technologies (including Software),Electronics,Energy,Environment,Healthcare,Manufacturing, including Industrial Biotechology

Description The UK supplier has actively marketed the Hi5 dual FIB-SIMS system as an industry first. This is highlighted in the Hiden Analytical publicity https://www.hidenanalytical.com/wp-content/uploads/2020/08/TDS-206-Hi5-SIMS-LR.pdf. This platform was also highlighted by the Hiden team promoting this innovative technology development at the SIMS Europe conference (https://www.hidenanalytical.com/events/sims-europe-2018-conference/). Hiden are also now marketing this simultaneous SIMS detector as a product for which quotes can be obtained (https://www.directindustry.com/prod/hiden-analytical/product-16750-2415369.html).
First Year Of Impact 2018
Sector Energy
Impact Types Economic

Description (EPISTORE) - Thin Film Reversible Solid Oxide Cells for Ultracompact Electrical Energy Storage
Amount € 4,599,129 (EUR)
Funding ID 101017709 
Organisation European Commission 
Sector Public
Country European Union (EU)
Start 01/2021 
End 12/2024
Description (HARVESTORE) - Energy HarveStorers for Powering the Internet of Things
Amount € 7,006,200 (EUR)
Funding ID 824072 
Organisation European Commission 
Sector Public
Country European Union (EU)
Start 12/2018 
End 11/2023
Description EPSRC ICSF Genesis
Amount £754,400 (GBP)
Funding ID EP/R024006/1 
Organisation Engineering and Physical Sciences Research Council (EPSRC) 
Sector Public
Country United Kingdom
Start 09/2017 
End 09/2020
Description Research Chair
Amount £255,000 (GBP)
Funding ID RCSRF2021\1243 
Organisation Royal Academy of Engineering 
Sector Charity/Non Profit
Country United Kingdom
Start 03/2021 
End 03/2026
Description SIMS-Europe 2018, Munster, Germany 
Form Of Engagement Activity A formal working group, expert panel or dialogue
Part Of Official Scheme? No
Geographic Reach International
Primary Audience Professional Practitioners
Results and Impact International conference on Secondary ion mass spectrometry (SIMS) 16th to 18th Sept 2018.
Presentation of two posters on 'High5'
EPSRC Strategic Equipment Fund : Grant of £1.8M: August 2017 for 3year project
2) Preliminary performance results for a new UHV SIMS, 'High5', with simultaneous positive and negative SIMS & ICP oxygen plasma source
Year(s) Of Engagement Activity 2018
Description UK Surface Analysis Forum, Harwell Materials Research Centre 
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 Talk on 'Simultaneous positive and negative SIMS with ICP plasma ion source': Talk to ~80 attendees covered most of the innovative
features of 'High5'. At this meeting RJC was presented with the 'Riviere Prize', an annual award from the UKSAF, the citation for this award
is 'This award is presented to researchers whose work has had a major impact on other researchers in the field of surface analysis'
Year(s) Of Engagement Activity 2018
Description Visit Research center I2CNER, Kyushu University, Japan 
Form Of Engagement Activity A talk or presentation
Part Of Official Scheme? No
Geographic Reach International
Primary Audience Other audiences
Results and Impact 1) Visit for 3 days to have collaborative interactions with Prof Tatsumi Isihara and Prof Maximoto group of workers in order to promote familiarity of High5 features & use of High5 in collaborative experiments during 2019/20
2) Seminar on High5 to ~60 staff at I2CNER
Year(s) Of Engagement Activity 2018