Correlative Analysis of Crystals in 3D
Lead Research Organisation:
University of Leicester
Department Name: Engineering
Abstract
The performance of any crystalline material depends greatly upon its crystal properties, such as crystallographic orientation. Crystalline materials include metals, alloys and ceramics, all of which are high-value strategically important materials. Materials characterisation is crucial to the understanding of key processes in a range of functional and structural materials that have applications across many industrial sectors. We request funding for a ZEISS Hercules package of CrystalCT and Crossbeam 350 with femtosecond (fs)-laser in correlative configuration, integrated and running on one powerful software platform. This new equipment represents a game changer for materials characterisation; it will enable numerous capabilities, including 3D non-destructive and high throughput crystallographic and microstructural imaging using laboratory-based X-ray source, access to deeply buried regions of interest as well as performing correlative analysis of crystals in 3D on large volumes of materials.
This equipment, a 3D crystallographic imaging system, will bring new capabilities to the Midlands region, becoming the only combination system in the UK capable of capturing isotropic voxel dimensions at sub-micron resolution, and will, for the first time, enable a transformative workflow for both multi-modal and multi-scale characterisation of crystalline materials, at length scale from centimetres to nanometres. The requested equipment has a strong demand at local, regional and national levels due to its unique capabilities for correlative 3D imaging of crystals. By working closely with multi-disciplinary research teams within the University of Leicester, and our regional and national partner organisations, we have identified three Core Areas with competitive regional and national strengths. It is anticipated that the proposed research topics that this equipment will support will be elevated to internationally competitive levels.
Micro-CT (also called micro computed tomography) is a 3D imaging technique that uses X-rays to look inside a material slice by slice. Absorption contrast tomography, the working principle describing how a conventional micro-CT works, measures density differences in a material, such as porosity, inclusions, defects, etc. However, it cannot not reveal the grain microstructure, defined by crystallographic orientations, which is key to almost any metallic materials' properties and performance. The combination of absorption and diffraction unravels a complete picture of grain microstructure which can then be linked to help researchers understand the defect formation mechanisms. In this sense, the stand-alone CrystalCT system is already an exceptional micro-CT. The unique correlative configuration of the CrystalCT and Crossbeam 350 with fs-laser is even more exciting as it enables the 3D grain imaging across the length-scales of centimetres to nanometres.
The equipment will be managed through a committee to oversee strategic issues, primarily focusing on making businesses aware of the research capabilities of this instrument, as well as growing a diverse and inclusive user base. Ultimately, supporting this equipment proposal will allow us to provide significant societal and economic benefit to the UK.
This equipment, a 3D crystallographic imaging system, will bring new capabilities to the Midlands region, becoming the only combination system in the UK capable of capturing isotropic voxel dimensions at sub-micron resolution, and will, for the first time, enable a transformative workflow for both multi-modal and multi-scale characterisation of crystalline materials, at length scale from centimetres to nanometres. The requested equipment has a strong demand at local, regional and national levels due to its unique capabilities for correlative 3D imaging of crystals. By working closely with multi-disciplinary research teams within the University of Leicester, and our regional and national partner organisations, we have identified three Core Areas with competitive regional and national strengths. It is anticipated that the proposed research topics that this equipment will support will be elevated to internationally competitive levels.
Micro-CT (also called micro computed tomography) is a 3D imaging technique that uses X-rays to look inside a material slice by slice. Absorption contrast tomography, the working principle describing how a conventional micro-CT works, measures density differences in a material, such as porosity, inclusions, defects, etc. However, it cannot not reveal the grain microstructure, defined by crystallographic orientations, which is key to almost any metallic materials' properties and performance. The combination of absorption and diffraction unravels a complete picture of grain microstructure which can then be linked to help researchers understand the defect formation mechanisms. In this sense, the stand-alone CrystalCT system is already an exceptional micro-CT. The unique correlative configuration of the CrystalCT and Crossbeam 350 with fs-laser is even more exciting as it enables the 3D grain imaging across the length-scales of centimetres to nanometres.
The equipment will be managed through a committee to oversee strategic issues, primarily focusing on making businesses aware of the research capabilities of this instrument, as well as growing a diverse and inclusive user base. Ultimately, supporting this equipment proposal will allow us to provide significant societal and economic benefit to the UK.
Publications
Sharma D
(2024)
Deposition behaviour of FeCrMnNiCo coatings deposited using mechanically alloyed powder: Comparing Cold Spray, HVOF, HVAF, and Laser Cladding processes
in Surface and Coatings Technology
| Description | The primary aim of the funding was to set up a facility comprising of two state of the art instruments using both X-rays and Electron microscopy to image microscopic features in 3D. These were selected to serve the needs of researchers both at University of Leicester and within UK Materials community, complementing existing research facilities both regionally and nationally. The facility is now up and running and routinely being accessed by researchers from within University of Leicester, with plans to train more researchers. Free access is being offered to PhD students and Early Careers Researchers (ECRs) in order to facilitate skill development and support pilot studies for future research grants. The instruments were selected with particular focus on a number of research themes, these being 1) Additive Manufacturing (AM), 2) Degradation in Structural Materials for Net Zero, 3) Planetary and other Materials. The facility has led to two external collaborations being established within themes 1) and 2). Firstly, a collaboration with Argonne National Laboratory (USA) surrounding the use of AM to replace wrought steel (316H) in nuclear reactors. Secondly, the UK Atomic Energy Authority has provided samples of a copper alloy that has been characterised with some of the unique capabilities of the new equipment, allowing us to visualise the crystallographic structure in 3D. This alloy is expected to have applications for thermal management in nuclear fusion reactors, being resistant to the harsh conditions caused by the plasma and thus understanding of this crystallographic structure is essential for modelling the long-term life of structural components. Both projects will improve knowledge around these materials to allow engineers to design safer, longer lasting and more cost-effective nuclear power stations. Further, work around Planetary Materials is gathering pace, building on Leicester's great heritage in Space and Planetary sciences. The Planetary Materials group has used the facility to analyse a number of extra-terrestrial materials including the Winchcombe meteorite and Martian nakhlite meteorites. The capabilities of the Hercules facility have allowed for detailed analyses of clay minerals in these samples, and by studying these, inferences can be made about water-rock interactions to better understand the geological processes that may have occurred in the early solar system. The facility has also enabled the preparation of samples for further analyses at a national facility, the electron Physical Science Imaging Centre (ePSIC) based at Diamond Light Source. Similar work on planetary materials is planned in the future for the joint NASA/ESA Mars Sample Return mission, with terrestrial analogues being analysed to determine their similarity to geological samples currently being collected by the Perseverance rover at Jezero Crater, Mars. |
| Exploitation Route | While the main focus has been on the above areas, the instruments have also provided some emergent opportunities for other research areas at Leicester, in particular within Bio-Engineering, Medical Sciences and Archaeology. While still in early stages, there are promising results on a number of projects that can be taken further. These include analysis of skeletal remains to understand the historic spread of leprosy, looking at the impact of novel breast and prostate cancer therapies on bone metastasis, and establishing the feasibility of 'avatar models' to develop treatments for patients with vision defects. External to Leicester, free access has also been extended to a number of academic institutes (Universities of Oxford, Loughborough, Southampton, Coventry, Nottingham, Bath) in order to support experiments. Work will continue with some of these partners with the staff and academics associated with the facility also seeking further collaboration both within the UK and further afield. |
| Sectors | Aerospace Defence and Marine Manufacturing including Industrial Biotechology Culture Heritage Museums and Collections Pharmaceuticals and Medical Biotechnology Transport |
| Description | Argonne National Laboratory - Characterisation of AM316H |
| Organisation | Argonne National Laboratory |
| Country | United States |
| Sector | Public |
| PI Contribution | Access to the new equipment has led to a collaboration with researchers at Argonne National Laboratory regarding additively manufactured 316H Stainless Steel (AM 316H SS). This steel crucial for nuclear applications due to its superior creep and corrosion properties at elevated temperatures. As additive manufacturing is a relatively new technique, the microstructural differences between traditional wrought and AM components is not as well understood. The Senior Experimental Officer has trained and supported a PhD student (funded as part of a partnership with Zeiss) to characterise a set of additively manufactured samples in different processing conditions via MicroCT. This has allowed detailed 3 dimensional, non-destructive characterisations of the defects arising due to creep testing and thus shed further insight into the differing creep behaviour of additively manufactured 316H stainless steel. Along with the expertise of the PI and additional supervisor based at Leicester, this has lead to a first publication, currently in draft. |
| Collaborator Contribution | Partners at ANL have provided a set of AM 316H SS samples that have undergone different processing conditions (as-built, solution annealed, stress relieved , hot isostatic pressing). These have been creep tested in two temperatures/loads conditions meant to mimic typical service conditions to allow the researchers to understand the differing failure as related to the processing conditions. Likewise, as agreed with the project team in the UK, they have also cut smaller samples from regions of interest in these test pieces to facilitate higher resolution MicroCT characterisation. They have also provided data sets of these creep tests to allow the PhD student to related their microstructural characterisation to the differing behaviours in the samples,. further enabling him to link this to theoretical behaviour. They have also provided comprehensive fractography and some EBSD data to support this and act as a starting point for more advanced characterisation in the UK |
| Impact | Invited talk at TMS 2025 - Xuan Zhang "Additive Manufacturing: Length-Scale Phenomena in Mechanical Response" |
| Start Year | 2023 |
| Description | University of Southampton - 3D crystallographic characterisation of Magnesium alloys |
| Organisation | University of Southampton |
| Country | United Kingdom |
| Sector | Academic/University |
| PI Contribution | The grant has allowed Leicester to provide free of charge access to the diffraction contrast tomography (DCT) enabled MicroCT in order to run a pilot study on magnesium alloys. The SEO'S expertise have been used to design and optimise the data collection along with initial data processing and reconstruction. As a result of a successful pilot study, further experiments have been conducted by the SEO, with Southampton making appropriate FEC contributions. A PhD student from Southampton has attended the facility to both understand the experiment and be trained by the SEO to allow independent data processing and to further their understanding of the fundamentals of the technique. Further experiments are planned for the near future with the FIB-SEM instrument in order to correlate with the existing data. |
| Collaborator Contribution | Southampton have provided expertise in modelling of grain growth behaviour in Magnesium alloys as well as suitable samples for the DCT experiment. Likewise, Dikai Guan acted as one of the speakers for the facility launch event described elsewhere. Once feasibility has been proven, financial contributions have been made at FEC for access to the instrument. |
| Impact | - |
| Start Year | 2023 |
| Description | Cosmic Coffee - Talk to local and SME industry |
| Form Of Engagement Activity | A talk or presentation |
| Part Of Official Scheme? | No |
| Geographic Reach | Regional |
| Primary Audience | Industry/Business |
| Results and Impact | Space Park Leicester hosts a regular event for local businesses, particularly SME in order to better network the academic and industrial communities. This is primarily aimed at better engagement, particularly to facilitate knowledge transfer. The Senior Experimental Officer gave a 10 minute talk covering the capability of both the new instrumentation and similar equipment already housed at Leicester, with a focus on how academics at the university could assist with a diverse set of engineering problems. |
| Year(s) Of Engagement Activity | 2024 |
| Description | Hercules Facility Launch Event |
| Form Of Engagement Activity | Participation in an activity, workshop or similar |
| Part Of Official Scheme? | No |
| Geographic Reach | National |
| Primary Audience | Other audiences |
| Results and Impact | A workshop was held at the University of Leicester to launch the new facility and bring together a diverse audience interested in the techniques facilitated by the new equipment. The aim was to break down barriers between different fields (e.g. Metals and Alloys, Geology, Planetary Science, BioMaterials, Archeology) in order to disseminate understanding and best practice, with the aim to generate new perspectives and foster cross disciplinary discussion and collaboration. This was facilitated by a number of talks during the morning from invited experts, drawn from both academia (Universities of Liverpool, Manchester, Southampton, Strathclyde, Swansea) and Industry (Carl Zeiss Ltd, XNovoTech, InformixPharma). Each session was finished with a panel discussion in which the speakers and audience could organically discuss key concepts and how they might be applied to different research problems. The day was concluded with a break out session in which attendees were asked to form small groups and discuss key questions around community engagement, current and future research challenges, and the technical capabilities required to over come these. There were between 50 and 60 attendees, with around half being external to University of Leicester. Notably, as well as academics and postgraduate students, there were a number of RTPs attending, including from Univ. of Warwick, Liverpool and Manchester. There was also involvement from industry, with attendees from Renishaw, Zeiss, Oxford Instruments, Silveray and Deben. Broadly the day was well received with a number of attendees expressing a desire to learn more about the techniques and incorporate them into their research. |
| Year(s) Of Engagement Activity | 2024 |
| URL | https://midlandsinnovation.org.uk/latest/events/university-of-leicester-hercules-facility-launch/ |
| Description | RMS IBM-FIG |
| Form Of Engagement Activity | A formal working group, expert panel or dialogue |
| Part Of Official Scheme? | No |
| Geographic Reach | National |
| Primary Audience | Postgraduate students |
| Results and Impact | The Royal Microscopical Society has a number of focused interest group in order to bring together experts in particular areas of microscopy. One of these, the Ion Beam Microscopy FIG has been established to cover aspects relating to focused ion beam microscopy, secondary ion mass spectrometry and other related techniques. This focus group aims to act as a focal point for these techniques in the UK (and limited international members) for examples arranging events such as the 'UK FIB & Prep Workshop', the 12th edition of which was held in January 2025, as well as provide expert advice in areas like roadmapping exercises. As a result in his participation with the Hercules facility, the SEO has been elected to the committee. |
| Year(s) Of Engagement Activity | 2024,2025 |