Strategic Equipment - a Dual Beam FIB/SEM with large area patterning, EBSD and nanoprobe capabilities

Lead Research Organisation: University of Oxford
Department Name: Materials

Abstract

The FIB/SEM instrument proposed combines various components to provide a powerful tool for a range of advanced nanoscale science. An accelerated ion beam focused to a spot size as small as 5 nanometres can be used to mill and slice materials with extreme precision, while an electron beam and various detectors provide means for nanoscale imaging and characterisation of the surfaces produced. A nanomanipulator probe allows samples to be rotated in-situ and for nanoscale slices of material to be lifted out for further study or use in devices.

We will use this instrument in two main ways:

1) Fabrication of micro-optical components

In Oxford we have in the past six years pioneered the use of focused ion beams to fabricate surfaces on materials such as fused silica or silicon with nanometre precision and sub-nanometre roughness. This allows us to create devices in which light is stored and manipulated with ultra-low scattering losses, and in which the interaction between light and matter is controlled with exquisite accuracy. We have already had considerable success with this technique on a small scale but are limited in the size of features we can produce. In this new instrument the sample can be moved with extremely high accuracy allowing larger surfaces to be patterned and enabling more complex and extended optical devices that reveal new physics and can be used as key components in a range of technologies. Photonics underpins a diverse range of industry in the UK and we anticipate that our work will lead to innovations in advanced information technologies and sensor systems for defence, healthcare and environmental monitoring, as well as the new field of Quantum Technologies in which the government is currently investing significant resources.

2) Characterisation of Materials

Oxford Materials department has long been a world-leading centre for materials characterisation, with particular contributions in electron microscopy and the microstructure of metals. It maintains a wide range of state-of-the-art instruments that are used both as high end scientific tools and as platforms for developing new techniques in microanalysis. This instrument will be used in both ways. It offers leading edge capabilities is 3D characterisation of material defects and impurities at the nanoscale that will enable new techniques aimed at understanding materials with unprecedented detail, and will be applied to solving key problems in the fields of nuclear materials, aerospace alloys, catalysis, and high temperature superconductors. Many of these projects are carried out in collaboration with industry, providing excellent routes towards commercial and societal impact as well as development of new knowledge. In collaboration with a local company (Oxford Instruments) we will try out prototype detector systems to accelerate instrument development and maintain our position at the forefront of this important field.

As well as the projects described above, a percentage of time on the instrument will be made available to outside users who will be able to find out about the instrument via our website and annual open days, and apply for instrument time to carry out their own research. The Oxford Materials department has extensive instrument support and user training programmes to ensure that all users can obtain the best from their instrument time. To ensure that the scientific projects pursued are of the highest quality, the use of the instrument and time allocation will be carried out by a steering board of experts who will meet at quarterly intervals.

Planned Impact

The immediate impact of the instrument will be to bring a new state of the art Materials Characterisation tool to the UK community. Through our shared usage policy and wide advertising of the instrument's capabilities, this will benefit both private and public sector organisations engaged in materials science research. The new techniques we are developing will also be made available through our training programmes thereby enhancing UK capabilities in FIB-based prototyping and in materials characterisation.
In the medium to long term the research programmes supported and enabled by the new instrument have potential for far-reaching impact on UK economic competitiveness, policymaking, and quality of life. Our programmes in structural metallics for nuclear and aerospace applications are carried out in close collaboration with industrial partners, so that progress made can feed rapidly through to improved performance of critical materials that impact UK (and worldwide) manufacturing. Improved alloys for aerospace reduce fuel demand and can play an important role in reducing the cost and environmental impact of aviation, with a global market for these materials estimated at US$15.3Bn (rnrmarketresearch.com). Nuclear materials enhance the safety and efficiency of fission reactors for public benefit, and the realisation of practicable designs for GENIV fission or future fusion reactors would transform the global energy landscape. Similarly our research projects on superconducting materials and catalytic nanomaterials have potential for significant commercial and societal impact, and are all closely linked to the strategic aims of our industrial partners. Improved understanding and processing of superconducting materials and systems will lead to advances in superconducting magnet technology and impact the performance and cost of instruments such as MRI scanners for healthcare, as well as research tools used in scientific laboratories around the world. The market size for superconductors was valued by Transparency Market Research at US$427M in 2013 and predicted to reach US$1.3Bn in 2020. Higher performance and better targeted catalytic materials lead to improvements in (for example) petroleum refining, vehicle emissions, hydrogen generation, and polymer manufacturing. The world catalyst market is currently US$16Bn, and predicted to grow to US$20Bn by 2018.
Quantum technologies are beginning to generate substantial commercial interest and although the current market is small, the field is viewed by many as having potential to transform all information-related fields, from sensing and detection (including imaging), metrology, communications, to computation. Major goals are perfectly secure communications (available in a limited sense now), improved clocks and cameras, and computers that can simulate complex molecules and perform calculations that classical computers would find intractably difficult. The new EPSRC funded Oxford-led Hub on Networked Quantum Information Technologies (NQIT) involves 20 industrial partners, including large international corporations such as Lockheed Martin and Raytheon and government agencies such as DSTL and NPL who seek both to guide components and systems to market and to use quantum technologies to enhance their businesses.
The optical device fabrication for which the proposed FIB will be used has potential for impact across the full range of technologies that NQIT is developing. A fully engineered light-matter interface can within the timescale of the project greatly enhance the capacity of the scalable quantum processor that is the main NQIT goal, and produce other (simpler) devices such as optical sensors that are of benefit to healthcare, defence and environmental monitoring. Single photon sources operating at ambient temperatures can benefit the York-led hub and their industrial partners, and can bring societal benefits by lowering the barrier to deployment of secure communications systems.

Publications

10 25 50
 
Description The focused ion beam / scanning electron microscope instrument was commissioned and set up in the David Cockayne Centre for Electron microscopy at the University of Oxford as intended, and is now being well-used for research in the department as described in the proposal and is available for use by others as part of the local characterisation facility. Leading UK company Oxford Instruments is making use of the instrument for the development of tools for 3D materials analysis. Much of the research carried out on the instrument so far has been in nanofabrication of optical components for quantum optics and optical sensing systems. The instrument offers unprecedented control and engineering of ultra-smooth surfaces at the micro/nano scale such that complex patterns can be produced for various device applications. Its capabilities are enabling a new spinout company, Oxford HighQ, which over the coming years will bring to market a new generation of sensors for applications including environmental monitoring and medical diagnostics.
The instrument is also being used for investigations in materials science. It has been central to a number of research results concerning zirconium alloys and some work on advanced characterisation via transmission Kikuchi patterns.
Exploitation Route Commercialised sensors by Oxford HighQ; Advanced patterning tools by partners FIBICS; 3D analysis systems by Oxford Instruments.
Sectors Aerospace, Defence and Marine,Agriculture, Food and Drink,Chemicals,Digital/Communication/Information Technologies (including Software),Electronics,Environment,Healthcare,Manufacturing, including Industrial Biotechology,Pharmaceuticals and Medical Biotechnology

 
Description The capabilities of the new FIB/SEM instrument were an important element in making the case for investment in new spinout company Oxford HighQ. We were able to use results from the instrument to demonstrate world leading fabrication capabilities and know-how that would form a key element of the company, and would allow the precision engineering of sensor instruments and devices where previous attemps to use optical microresonators in industrial sensors have failed. The instrument is now used regularly by Oxford HighQ on a commercial basis to produce components for the sensors that it is developing, and components for supply to external groups. The company has hired and trained one full time engineer to work on fabrication who is the main user of the instrument, and has recently also begun paying for time of a university technician to perform some of the routine fabrication work. 2022 update - Oxford HighQ's first product, a laboratory instrument for measuring drug loading on nanoparticles for use in pharmaceuticals R&D, is in the beta phase and a product launch is planned for September this year. The microcavities fabricated using the Crossbeam FIB are at the heart of thiese instruments, which will bring new capabilities to pharmaceuticals labs developing drugs that utilise nanoparticle delivery methods. The instrument is also used on a wider commercial basis, primarily through Oxford Materials Characterisation Service (OMCS). For example in the 20 months to March 2022 OMCS has used 63.5 hrs of Crossbeam time working on commercial contracts for predominantly four customers and with a commercial value of £15,875, on the following topics: i) Micromachining a variety of structures for nanomaterials characterisation ii) FIB and subsequent SEM imaging of corrosion layers for an energy company iii) FIB and subsequent SEM analysis of carbon/silicon composite anodes for lithium ion batteries iv) FIB and SEM imaging of biocomposite materials.
First Year Of Impact 2018
Sector Manufacturing, including Industrial Biotechology
Impact Types Economic

 
Description EPSRC standard grant
Amount £1,412,712 (GBP)
Funding ID EP/R009392/1 
Organisation Engineering and Physical Sciences Research Council (EPSRC) 
Sector Public
Country United Kingdom
Start 12/2017 
End 12/2020
 
Description Horizon 2020 ERA-NET QuantERA (cofund)
Amount £1,311,422 (GBP)
Funding ID EP/R044058/1 
Organisation Engineering and Physical Sciences Research Council (EPSRC) 
Sector Public
Country United Kingdom
Start 02/2018 
End 01/2021
 
Description Technology programme
Amount £875,151 (GBP)
Funding ID EP/R045232/1 
Organisation Engineering and Physical Sciences Research Council (EPSRC) 
Sector Public
Country United Kingdom
Start 01/2018 
End 03/2019
 
Description Understanding the effect of CW on SCC of PWR components
Amount £234,698 (GBP)
Organisation Électricité de France EDF 
Sector Private
Country France
Start 10/2023 
End 03/2027
 
Description Collaboration with Lidzey and Tartakovskii groups on strongly coupled 2D materials 
Organisation University of Sheffield
Country United Kingdom 
Sector Academic/University 
PI Contribution Fabrication of open microcavity substrates for experiments
Collaborator Contribution Partners lead the experiments
Impact 10.1038/NPHOTON.2017.125 10.1038/s41467-018-07249-z 10.1088/2053-1583/abc5a1
Start Year 2013
 
Description Collaboration with Shanghai University 
Organisation Shanghai University
Country China 
Sector Academic/University 
PI Contribution We have hosted visitors from Shanghai University during 2019 where they have familiarized with our unique high-resolution characterization methodology. They have characterized samples from our collaborative projects and learn how to analyse the data. This will be the basis for future joint publications and joint projects.
Collaborator Contribution As an International Expert Group Member of Shanghai University, I visit China twice per year. During my visits we discuss current and future collaborations and review joint publications. At present, three manuscript have been prepared and submitted to international journals. The topics covered were already presented at international conferences (e.g. Int Symp on Environmental Degradation of Materials in Nuclear Power Systems)
Impact Joint contributions to the 19th Int Symp on Environmental Degradation of Materials in Nuclear Power Systems: -Coupling effect of charged-hydrogen and cold work on oxidation behavior of 316L stainless steel in deaerated high temperature water -Characteristics of oxide films formed on 309L and 308L stainless steels in simulated PWR primary water -Diffusing hydrogen effect on the oxide film on 316L SS in simulated PWR secondary side water -Stress corrosion cracking of stainless steel cladding layers in simulated PWR primary water -Effect of post weld heat treatment on microstructure and PWSCC of Alloy 52M weld metal in dissimilar metal weld joint -Effect of weld dilution and dendrite orientation on PWSCC behavior of Alloy 52M weld metal -Microstructural Evolution of 52M weld metal near the fusion boundary and oxide films formed in simualted PWR primary water
Start Year 2019
 
Description DSTL sensing 
Organisation Defence Science & Technology Laboratory (DSTL)
Country United Kingdom 
Sector Public 
PI Contribution Development of sensing technology
Collaborator Contribution Financial support via an iCASE studentship
Impact No outcomes yet.
Start Year 2020
 
Description FIBICS patterning collaboration 
Organisation Fibics Incorporated
Country Canada 
Sector Private 
PI Contribution Development of software for the generation of stream files for control of focused ion beam instruments. Input on required hardware specifications and parameter control for precision surface fabricationo using FIB instruments.
Collaborator Contribution FIBICS (http://www.fibics.com/) are world leading commercial developers of applications in focused ion beam microscopy. As part of this they develop control systems (computing systems and software) for focused ion beam instruments, specialising in beam control and patterning. Their interest in partnership is in developing products optimised for precision fabrication
Impact None yet.
Start Year 2016
 
Description Oxford Instruments Crossbeam 
Organisation Oxford Instruments
Country United Kingdom 
Sector Private 
PI Contribution Provision of access to Crossbeam FIB/SEM for the development of 3D analytics. So far we have provided 3-4 days access to the instrument for Oxford Instruments, and 2 x 4 days access to Zeiss applications personnel.
Collaborator Contribution Development of 3D EBSD/EDX software
Impact None yet
Start Year 2016
 
Description Photonic Bose Einstein condensates 
Organisation Imperial College London
Department Department of Surgery and Cancer
Country United Kingdom 
Sector Academic/University 
PI Contribution Fabrication of mirrors for microscopic cavities for photonic BECs
Collaborator Contribution Experimental realisation of photonic BECs
Impact None yet
Start Year 2015
 
Description Quantum well polaritons 
Organisation University of Sheffield
Department Florey Institute
Country United Kingdom 
Sector Academic/University 
PI Contribution Fabrication of mirrors for quantum well polariton experiments
Collaborator Contribution Carrying out low temperature experiments on exciton polaritons to explore fundamental condensed matter physics and possible device applications
Impact 10.1103/PhysRevLett.115.246401 10.1063/1.5019933
Start Year 2013
 
Description UTA Nanoholes for protein measurements 
Organisation University of Texas at Arlington
Department Department of Bioengineering
Country United States 
Sector Academic/University 
PI Contribution We have fabricated nano-apertures in gold films that allow single proteins to be trapped and observed using laser transmission experiments
Collaborator Contribution The UTA group perform the trapping and measurement experiments to study protein dynamics
Impact None yet
Start Year 2016
 
Company Name Oxford HighQ Ltd 
Description Oxford HighQ will develop and market sensors and analytics instruments for chemicals and nanoparticles in fluids, using a novel optical microresonator technology that provides high sensitivity detection capabilities requiring only minute (sub-nanolitre) fluid quantities. These devices will fulfil unmet needs in a range of markets including materials R&D, biomedical sciences, environmental monitoring, security and healthcare. The company will also bring to market precision micro-optical components such as micromirrors to support photonics R&D and the emerging quantum technologies sector. The company incorporated as a spin-out from the University of Oxford in October 2017. At the time of writing (March 2018) it is negotiating seed funding. 
Year Established 2017 
Impact No achievements yet. The company will initially employ three full time engineers.
Website http://www.oxfordhighq.com
 
Description Interview for French national news 
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 Industry/Business
Results and Impact In Dec 2019 I was awarded the first Excellence in Nuclear Reactor Science in the UK Award by Framatome. The ceremony took place in the French Embassy in London and I was interviewed by the French TV, by Framatome for their podcast and by the written press. Extracts from these interviews can be found in YouTube, Facebook, LinkedIn, etc. I talked about our advances in understanding materials properties and problems by looking at atoms and how important the contribution from academia was for such important industrial challenges.
Year(s) Of Engagement Activity 2019
URL https://www.youtube.com/watch?v=sY739SUBgY4
 
Description School Visit (Botley School, Oxford) 
Form Of Engagement Activity A talk or presentation
Part Of Official Scheme? No
Geographic Reach Local
Primary Audience Schools
Results and Impact Y3 students were introduced to Microscopy and Exploring the Nanoworld as part of the Science Week (STEM). Around 60 students plus teachers were present. I used a presentation with videos and pictures from my research (nuclear energy, catalyst nanoparticles and sample preparation for electron microscopy). Importance of understanding materials by looking at atoms was explained. A 30 min discussion with Q&A followed. The students engaged well and have been asking questions ever since. A 2nd visit this year has already been planned.
Year(s) Of Engagement Activity 2019
 
Description Talk to university admin staff 
Form Of Engagement Activity A talk or presentation
Part Of Official Scheme? No
Geographic Reach Local
Primary Audience Industry/Business
Results and Impact The University of Oxford organizes staff team days where they become familiar with aspects of the university that they are not usually exposed to, for example research. This year, I was invited to talk about my group research and I chose the topic of "Understanding degradation of materials in nuclear reactors". I expanted the topic so that the audience could also appreciate how our characterization techniques allowed the understanding of "big" problems by looking at "small" volumes (where atoms are observed directly). I believe the audience enjoyed it very much, since there were many questions afterwards and, as a result, many members of the admin team now recognize me and my research and told me they feel more engaged and "valued".
Year(s) Of Engagement Activity 2019
 
Description UK Quantum Technologies Showcase 2017 and BBC Click appearance 
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 A team from Jason Smith's group took a demonstrator instrument to the UK Quantum Technology Showcase 2017 at the QE2 centre in London. The demonstrator used optical microresonators to trap and measure nanoparticles approximately the size of flu virus particles diffusing in a fluid. The exhibit, entitled "catching the flu" enabled visitors to tune the resonator relative to a in incident laser beam such that the trapping worked when the leaser coupled into the cavity. Participants could the see the response of the mode to individual nanoparticles on an oscilloscope. The exhibit also featured an animation showing a future application of the instrument as a point of care medical diagnostics system. The purpose of the exhibit was to show off the technology we are developing and to advertise the spinning out of a new company Oxford HighQ which will bring the technology to market. The showcase event was attended by professionals, business leaders, investors, media and government figures. we were fortunate to be interviewed by the BBC Click team and our short interview was included in the January 5 edition named "Quantum at Solstice". The Youtube version of this has been viewed some 160,000 times.
Year(s) Of Engagement Activity 2017
URL https://www.youtube.com/watch?v=7HXTt7HMDE8
 
Description Undergraduate demonstration of TEM capabilities 
Form Of Engagement Activity Participation in an open day or visit at my research institution
Part Of Official Scheme? No
Geographic Reach Local
Primary Audience Undergraduate students
Results and Impact Every year I organize demonstrations in our research labs to familiarized groups of interested undergraduate students with our rearch projects. I use the characterization of cracks in nuclear reactor materials as they are perfect to illustrate how the failure of a several tonnes component can be understood by looking at the changes of a few atoms around a crack tip. All students are enrolled in our Materials Science undergraduate degree and the main purpose of this activity is to establish tangible links between the topics they study in their lectures and lab practicals and the "real" research that goes on in the department (most of the time, unnoticed by them). The outcome is always very rewarding, since I schedule the demo for 1.5h per group, but the number of questions and requests aftwerwards easily take the session beyond the 2h duration. Many of the undergraduate students will hopefully be interested enough in my research area to apply for a DPhil project in my group.
Year(s) Of Engagement Activity 2018,2019