A LEAP 5000 XS for the UK National Atom Probe Facility

Lead Research Organisation: University of Oxford
Department Name: Materials


This proposal is to install a state-of-the-art Local Electrode Atom Probe (LEAP) 5000 XS at the University of Oxford. Atom probe tomography (APT) is a type of microscopy that provides unique insight into 3D atomic distributions within materials at a scale that even the most advanced electron microscopes cannot routinely achieve. Hence APT is now an indispensable materials characterisation tool used in major international materials laboratories around the world.

The APT technique was pioneered in the UK, and for the past 30 years the Oxford Atom Probe Laboratory, a unique national facility, has maintained an international reputation for highly innovative APT research. The need for atomic-scale microstructural information is increasingly important for the design and development of the next generation of higher performance materials and devices. Hence, the unique insights provided by APT have become essential to advance understanding within a steadily increasing number of research programmes around the UK.

The two atom probe instruments installed at Oxford currently serve the research needs of the entirety of UK academia and industry. However, the older of these instruments is now no longer technologically sustainable and must be decommissioned. Hence, a new atom probe is urgently required to meet the current, and increasing, access demands for APT and to keep the UK competitive across a variety of key materials research topics. The main outcome of this proposal will be continuing to increase visibility of and access to APT for researchers around the UK.

The LEAP 5000 XS will allow us to address key analytical problems and generate greater impact in projects of strategic importance in the research groups of academic staff at Oxford and our Co-Is at universities, as well as working on projects with a wide range of industrial partners. The specific themes we will work on will use the LEAP 5000 XS to contribute to the development of novel materials across a wide range of applications, including efficient green energy materials, aerospace and automotive alloys, and even bio-implants, and to assist UK industry to maintain competitiveness and grow market share.

Planned Impact

The LEAP 5000 XS will underpin research into real world problems in design and manufacture of new materials and devices across a wide range of applications, under a variety of EPSRC themes, such as Physical Sciences, Manufacturing the Future, Healthcare Technologies, Engineering and Energy. This highlights a key reason for the recent growth in influence and impact of APT, which is a rapid broadening in the range of research topics to which it is being applied. This is evident in the emergence of cross-disciplinary applications, such as the enthusiastic uptake of the technique by the international Geological Sciences community and emerging interest demonstrated by the Biological/Medical Sciences. APT has potential to provide completely new perspectives on critical science in these fields.

A central feature of our vision for the new instrument is that it will deliver important new results and understanding to university partners and their industrial collaborators. This is not an activity that will have to be built up from scratch, as the investigators already hold a substantial portfolio of projects funded by UK industry, but the range, depth and significance of the output on problems that are both scientifically extremely challenging and of direct and immediate commercial relevance will be substantially increased by the requisite availability of this genuinely state-of-the-art machine. With academic partners, we will continue to generate impact by output of first class papers in the scientific literature.

Access to the new LEAP 5000 XS will also benefit researchers at earlier stages of their academic careers, ensuring adequate access for them to explore ambitious lines of new APT-based research. An emphasis will be placed on training. Ongoing users of the new instrument will be trained to an expert level in all aspects of the technique so as to understand the strengths and limitations when interpreting results from the perspective of their own materials investigation. Hence it will play a role in training and development for many in the next generation of students and ECRs who will take up roles in UK academia and industry leading scientific research in a diverse range of fields. This is critically important in fields such as nuclear research where there is an emphasis on re-establishing technical competency and international leadership.

More than 10 companies are actively involved in projects specifically outlined in this proposal. As the letters of support demonstrate, these collaborators share the ambition to use the LEAP 5000 XS to contribute to the development of next-generation materials across a wide range of engineering themes. Partnerships such as the Rolls Royce and Constellium University Technology Centres represent significant investment by EPSRC and industry to support multi-institutional collaborative research with the potential for immediate real-world impact to manufacturing in the UK and contribute to specific EPSRC priority areas such as: Lightweight Systems, Materials Characterisation and Structural Integrity and Materials Behaviour.

Examples of projects that we plan to undertake with these industrial partners are in the power generation, semiconductor materials, catalysis, aerospace and automotive sectors. UK industry has a leading position in many of these areas and must maintain competitiveness and grow market share. Some of these sectors are extremely large, for example, silicon PV alone is a $100bn global industry. Furthermore, we are continually in discussion with new partners who have problems that will benefit from the access to unique insights offered by the new instrument. One main impact of this project is to ensure that academia and industry has access to competitive facilities within the UK. Without this, there is real risk that industrial partners could move entire projects, not just the APT aspects, to international competitors who are actively installing similar facilities.


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Gault B (2021) Atom probe tomography. in Nature reviews. Methods primers

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He H (2021) Atom Probe Tomography of a Cu-Doped TiNiSn Thermoelectric Material: Nanoscale Structure and Optimization of Analysis Conditions. in Microscopy and microanalysis : the official journal of Microscopy Society of America, Microbeam Analysis Society, Microscopical Society of Canada

Description The role of the LEAP 5000XS is to facilitate innovative research across the broadest possible materials research. Key findings include -

Geological Materials
Using a combination of simulated data and pyrite isotopic reference materials, a methodology has been developed to obtain quantitative relative sulfur isotope measurements from atom probe tomography (APT) datasets. This capability is important for e.g. understanding the history of geological materials. This study builds on previous attempts to characterize relative 34S/32S ratios in gold-containing pyrite using APT. By analyzing against a standard material, acquired under similar conditions, we have extracted d34S values to within ±5‰ (1‰ = 1 part per thousand) of the published values of our standards.

Superconductor Materials
there has been an increasing effort in improving the performance of Nb3Sn superconductor materials for high-field applications, in particular for the fabrication of components suitable for the realization of the Future Circular Collider (FCC) at CERN. This challenging task has led to the investigation of new routes to advance the high-field pinning properties. The effect of hafnium addition to the standard has been recently demonstrated to be particularly promising in other materials and, in this research, we investigated the origins of the observed improvements of the superconducting properties in Nb3Sn. Atom Probe Tomography (APT) characterization clearly show that, in presence of oxygen, both fine Nb3Sn grains and HfO2 nanoparticles form. Although EXAFS is unable to detect significant amounts of Hf in the A15 structure, APT does indeed reveal some residual intragrain metallic Hf. Correlation to material performance show that the improvements generated by Hf addition can significantly enhance the high-field performance, bringing Nb3Sn closer to the requirements necessary for FCC realization.

Thermoelectric Materials
Cu-doping and crystallographic site occupations within the half-Heusler (HH) TiNiSn, a promising thermoelectric material, have been examined by atom probe tomography. Research show that experimental conditions could signifcantly effect the results of the characterisation experiments. The outcome of this work show that the experiment can be appropriately calibrated for the analysis of these materials, such that APT can provide atomic-scale information to guide refinement of the manufacturing of these thermoelectric components with optimised performance.

Al alloys for Automotive Components
Aluminium alloys are seeing wider use in the automotive sector as part of a drive to reduce vehicle weight and improve energy efficiency. In this study two variants of a high
strength Al-6xxx alloy were investigated; one with a low Cu content, the other with a high Cu content. Focussing on rthe very earliest stages of solute clustering, the research provided greater understanding of the mechanisms governing precipitation after natural ageing and the effect Cu content has on this precipitation, in relation to improving mechanical properties for automotive crash management systems. The ageing process for the investigated alloy involves two stages of raised temperature ageing; a lower temperature pre-age and a higher temperature final age. The new insights can inform the manufacturing to develop more effective, energy efficient, and greener processing routes.

Quantum dots
We investigated metal-organic vapor phase epitaxy grown (InGa)(AsSb)/GaAs/GaP Stranski-Krastanov quantum dots (QDs) with potential applications in QD-Flash memories by cross-sectional scanning tunneling microscopy (X-STM) and atom probe tomography (APT). We demonstrated that the combination of X-STM and APT is a very powerful approach to study semiconductor heterostructures with atomic resolution, which provides detailed structural and compositional information on the system. APT experiments revealed that the QDs are GaAs rich with smaller amounts of In and Sb. This confirms that the InGaSb and GaAs layers involved in the QD formation have strongly intermixed. A detailed analysis of the QD capping layer shows the segregation of Sb and In from the QD layer, where both APT and X-STM show that the Sb mainly resides outside the QDs proving that Sb has mainly acted as a surfactant during the dot formation. Our structural and compositional analysis provides a valuable insight into this novel QD system and a path for further growth optimization to improve the storage time of the QD-Flash memory devices.
Exploitation Route Other researchers can either directly build upon the foundations provide by the specific outcomes described above or may be motivated by the successful APT analyses to plan to utilise the LEAP 5000XS facility to generate unique new atomic-scale to inform their own materials research problems.
Sectors Aerospace, Defence and Marine,Electronics,Energy,Environment,Manufacturing, including Industrial Biotechology,Other

Description One of the goals of the LEAP 5000XS was to enable atomic-scale investigations to a much wider range of materials. To this end the facility has initiated and underpinned ongoing new research in fields of - geological materials, superconductors, nanoelectronics, light weight automotive components. Significantly, the LEAP 5000XS has been incorporated into the Royce Institute, with students from around the UK able to bid for funded and fully-supported access to this instrument to underpin their research. To this end, as part of the Royce Institute the facility has supported a wide range of new investigations from researchers at Universities of Sheffield, Brunel, Cambridge, Southampton, Manchester, Nottigham and Glasgow
First Year Of Impact 2020
Sector Aerospace, Defence and Marine,Education,Electronics,Energy,Environment,Manufacturing, including Industrial Biotechology,Other
Impact Types Societal,Economic

Description An Atomic-Scale Characterisation Facility for Active Nuclear Materials
Amount £3,822,136 (GBP)
Funding ID EP/T011505/1 
Organisation Engineering and Physical Sciences Research Council (EPSRC) 
Sector Public
Country United Kingdom
Start 11/2019 
End 03/2023
Description EPSRC CASE Studentship - A Akinwale
Amount £30,000 (GBP)
Organisation Constellium 
Sector Private
Country France
Start 10/2021 
End 10/2025
Description Ni-based ODS alloys for Molten Salt Reactors
Amount £499,728 (GBP)
Funding ID EP/T002441/1 
Organisation Engineering and Physical Sciences Research Council (EPSRC) 
Sector Public
Country United Kingdom
Start 08/2019 
End 08/2022
Description Simultaneous Corrosion/Irradiation Testing in Lead and Lead-Bismuth Eutectic: The Radiation Decelerated Corrosion Hypothesis (RC-3)
Amount £543,314 (GBP)
Funding ID EP/T002808/1 
Organisation Engineering and Physical Sciences Research Council (EPSRC) 
Sector Public
Country United Kingdom
Start 09/2019 
End 09/2022
Description DA MacLaren 
Organisation University of Glasgow
Country United Kingdom 
Sector Academic/University 
PI Contribution Development of APT techniques for the atomic-scale characterisation of thermoelectric materials
Collaborator Contribution Development of novel Half-Heusler thermoelectric materials
Impact https://doi.org/10.1017/S1431927621012162
Start Year 2020
Description Geological materials 
Organisation University of Leoben
Country Austria 
Sector Academic/University 
PI Contribution APT provided atomic-scale characterisation of a range of geloogical materials
Collaborator Contribution Collaborators led the research into a vareity of gelogical materials, with relvance to mining and/or specimen dating
Impact https://doi.org/10.1017/S1431927621013568
Start Year 2019
Description M A Auger 
Organisation Charles III University of Madrid
Country Spain 
Sector Academic/University 
PI Contribution Enabled atomic scale analyses of irraidated ODS steels, and other steels, with applications to the build of fission and fusion reactors
Collaborator Contribution Development of the next generation of high performance steels for a variety of applications as components of nuclear reactors
Impact https://doi.org/10.1016/j.jnucmat.2021.152842 https://doi.org/10.1016/j.mtla.2020.100946 https://doi.org/10.1016/j.jnucmat.2020.152466
Start Year 2019
Description Nb3Sn superconductors 
Organisation Florida State University
Country United States 
Sector Academic/University 
PI Contribution Developed APT techniques for atomic scale characterisation of superconductor materials
Collaborator Contribution developed cutting edge Nb3Sn superconductor materials
Impact https://doi.org/10.1038/s41598-021-97353-w
Start Year 2019
Description Quantum Dots 
Organisation Eindhoven University of Technology
Country Netherlands 
Sector Academic/University 
PI Contribution APT provided 3D chemically-resolved atomic scale characterisation of (InGa)(AsSb)/GaAs/GaP Stranski-Krastanov quantum dots
Collaborator Contribution Collaborators designed and processed the (InGa)(AsSb)/GaAs/GaP Stranski-Krastanov quantum dots. They undertook complementary microstructural characterisation .
Impact https://doi.org/10.1038/s41377-021-00564-z
Start Year 2020
Description Virtual Atom Probe Tomography and Microscopy Conference 
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 The Virtual Atom Probe Tomography and Microsocpy Conference is the most prestigious international conference dedicated to materials research underpinned by APT. More than 200 researchers from around the worls attended this 3-day event which was held via Zoom and streamed on Youtube. The event raised the profile of the new atom probe facility within this research community. As part of the conference delegates, in paerticular students, were encouraged to pre-record 5 minute mini-presentations to highlight their research which we then posted on youtube. We received 44 submissions which have been collectively received over 4,300 views.https://www.youtube.com/playlist?list=PL-0gZJOh94SfNCVFaZm6WNGLc2BDkvRex
Year(s) Of Engagement Activity 2020
URL https://aptm2020.web.ox.ac.uk/