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Operando XRD mapping experiment at ESRF for the FutureCat project

Photo of Dr Stephen Price and Dr Ashok Menon at ESRF experiment

Image credit: Harry Gillions (WMG)

 

Our Senior Scientist Dr. Stephen Price, with Dr. Ashok Menon and Harry Gillions from collaborator institute WMG, University of Warwick completed a beamtime in May at ESRF.  They set up an operando XRD mapping experiment on multilayer pouch cells fabricated at the WMG battery scale up pilot line to understand their degradation modes.

Stephen has been studying X-ray diffraction computed tomography (XRD-CT) and mapping techniques to provide direct quantification of performance of real world battery operation without the need to extrapolate from model cells. He is looking to devise non-destructive techniques to rapidly benchmark industry-relevant large-format cells, such as those manufactured at WMG, and further develop the operando methods that can be applied to study battery degradation that occur with long-term cycling. These findings can be translated  back to  WMG , and then to the broader industry to build better batteries.

ID31 at ESRF has the required combination of hardware, software and expertise to be able to run this experiment.

 

It was great to work with the battery development experts at WMG, combining our knowledge to push the operando imaging capabilities to see inside ever larger and more commercially relevant batteries. ~ Dr. Stephen Price

Finden partnered with University of Sheffield and WMG as part of FutureCat Phase II activities, led by Prof Louis Piper at WMG to work on the Faraday Institution’s collaborative project along with eight other industrial partners, eight other academic partners and two national research facilities. They aim to create the future lithium-ion cathode materials for electric vehicles.

Working with Finden has enabled us to develop spatial mapping of the intercalation reactions in real time in our pilot line pouch cells, which has helped accelerate both active material and cell designs. ~ Prof. Louis Piper

Latest work exploring the use of the ProxSkip algorithm 

Comparison Proxskip diagram

We are excited to share our latest work exploring the use of the ProxSkip algorithm as an efficient solution for accelerating iterative methods in imaging inverse problems. This project was led by our Senior Research Scientist Evangelos Papoutsellis, in collaboration with Kostas Papafitsoros (Queen Mary University) and Zeljko Kereta (University College London). By randomly skipping regularisation steps, ProxSkip significantly reduces computational time without compromising convergence. We also introduce a novel variant, PDHGSkip, which further enhances performance. Extensive numerical experiments demonstrate that these methods deliver faster computations while maintaining high-quality reconstructions.

We acknowledge funding from from the Analysis for Innovators (A4i) Denoising of chemical imaging and tomography data project, in collaboration with National Physical Laboratory  which supported early development. As part of this effort, we also extended the stochastic optimisation framework in the Core Imaging Library (CIL) to incorporate these new algorithms. We are pleased to announce that this work has been accepted for presentation at the 10th International Conference on Scale Space and Variational Methods in Computer Vision (SSVM2025). For more information, we refer to the preprint version https://arxiv.org/abs/2411.00688.

PhD student Antonia Bobitan completed 2nd beamtime of year for STORMING at DESY

Photo of DESY team for Storming April beamtime

Our PhD student Antonia Bobitan recently completed her 2nd beamtime of the year for STORMING. This time on beamline P21.2 at DESY, where she performed an in situ XRD-CT experiment on 3D-printed monoliths along with collaborators Dr. Matthew Potter (Bath), Maciej Walerowski (Southampton) and Dr. Lucy Costley-Wood (UCL). The team successfully tested our newly designed reactor and generated lots of nice images.

Successful beamtime for the STORMING project at the ESRF Beamline BM31 in Grenoble, France

Photo of ESRF experiment set up

Our PhD student Antonia Bobitan took part in a beamtime on beamline BM31 at ESRF in March with Prof. Andrew Beale and Dr. Yaroslav Odarchenko. They joined forces with Maria Asuncion Molina Esquinas from UCL. Antonia performed a combined XAFS/XRD operando experiment on our STORMING catalysts for CH4 conversion to high-purity H2 and CNTs. She is looking forward to spending the next few months analysing the large amount of data this successful experiment generated!

Spatial and Temporal Visualization of Polymorphic Transformations in Pharmaceutical Tablets

Graphical abstract

Our Senior Scientist Stephen Price has been working with Julia Gasol Cardona, Iain Oswald (University of Strathclyde), Daniel Markl (CMAC), Andy Maloney (CCDC – The Cambridge Crystallographic Data Centre), and teams at DESY, ELDICO Scientific AG and ESRF – The European Synchrotron on a project where X-ray Diffraction Computed Tomography (XRD-CT) has been used to reveal pressure-induced phase transformations in pharmaceutical tablets of glycolide as a function of compaction pressure. This novel application of the XRD-CT methodology enables non-destructive molecular level insight and is a step change in the way we are able to view formulated products. In the broader context of pharmaceutical research, the application of this methodology to pharmaceutically relevant systems will enable a deeper understanding of the effect of tableting pressure on the formulation in pharmaceutical products. Read the article at https://doi.org/10.1002/anie.202412976

4th STORMING Consortium Meeting in London

Photo of attendees at Storming Meeting London 11 Sep 2024

We were proud to host the 4th STORMING Consortium Meeting in London on the 11th & 12th September. It was wonderful to meet up with the consortium members and share new insights on the project.

STORMING will develop breakthrough and innovative structured reactors heated using renewable electricity, to convert fossil and renewable CH4 into CO2-free H2 and highly valuable carbon nanomaterials for battery applications. Find out more at https://storming-project.eu

Thank you to everyone for attending!

Obtaining parallax-free X-ray powder diffraction computed tomography data with a self-supervised neural network

Finden’s latest work with UCL Chemistry, Deutsches Elektronen-Synchrotron DESY, Dyson School of Design Engineering at Imperial College London and Science and Technology Facilities Council (STFC) has been published in a new paper by Hongyang Dong “Obtaining parallax-free X-ray powder diffraction computed tomography data with a self-supervised neural network” in npj Computational  Materials.  This study introduces a method designed to eliminate parallax artefacts present in X-ray powder diffraction computed tomography data acquired from large samples. These parallax artefacts manifest as artificial peak shifting, broadening and splitting, leading to inaccurate physicochemical information, such as lattice parameters and crystallite sizes. Our approach integrates a 3D artificial neural network architecture with a forward projector that accounts for the experimental geometry and sample thickness. It is a self-supervised tomographic volume reconstruction approach designed to be chemistry-agnostic, eliminating the need for prior knowledge of the sample’s chemical composition. We showcase the efficacy of this method through its application on both simulated and experimental X-ray powder diffraction tomography data, acquired from a phantom sample and an NMC532 cylindrical lithium-ion battery.

Film about our RSC Chemistry Horizon Sir George Stokes Prize

The Royal Society of Chemistry made a short film to celebrate our Royal Society of Chemistry Horizon Sir George Stokes Prize with Sciad Communications and Cambridge FilmWorks. The piece was filmed at the Research Complex at Harwell, Rutherford Appleton Laboratory and our joint recipients at the Deutsches Elektronen-Synchrotron DESY in 2023. Here we speak about our work on the development and application of X-ray diffraction computed tomography to image and identify structure-activity relationships within functional materials and devices. Click on the image below to watch the film.

Read more about our work with chemical imaging and tomography.

Our Chemical Imaging and Tomography training course 2024 is complete

Photo of Training Course 2024 Lectures

Our Chemical Imaging and Tomography training course in collaboration with The University of Manchester is complete and we’ve had a wonderful time with our participants.

Over the course of three days, our expert instructors guided learners through a comprehensive overview of this cutting-edge technology. 

Students learned the fundamental principles, covering current instrumentation, and how these approaches are applied using the scattering and spectroscopic methods with emphasis on X-ray diffraction computed tomography (XRD-CT). In addition, our participants were introduced to XRD-CT data processing and analysis using Python, a powerful tool for interpreting chemical imaging data. 

By the end of the course, they had new-found confidence to apply these skills to their own research. 

Thank you to all of our amazing graduates. We were so impressed by the progress you made and we can’t wait to see the work you’ll accomplish with your newfound knowledge and skills!

Photo of Training Course 2024 Group

Happy International Women’s Day

Antonia Bobitan photo at DESY Feb 2024We are so proud of our WomenInSTEM for their work with us at Finden.

We would like to feature Antonia Bobitan our PhD student who has just completed experiments for her Storming EU Project at the DESY synchrotron.

“We’ve been doing some pretty cool stuff here at DESY beamlines P21.2 and P07, from magnetic induction heating to in situ XRD-CT of batteries.

For the Storming EU Project, we (FINDEN LTD, UCL) have successfully performed in situ/operando XRD experiments of CH4 conversion to H2, demonstrating the power of the Fe-based catalysts made by University of Bologna (Alma Mater Studiorum – Università di Bologna)!

I’m a person that’s environmentally conscious so I figured this degree would also create some opportunities for me to be involved in the fight against climate change. And it has, especially with the PhD project, which is all about creating carbon-negative H2 in order to reduce our fossil fuel usage.”

Congratulations and keep up the hard work Antonia!


The project STORMING has received funding from the European Union’s Horizon Europe Research and Innovation Programme, under Grant Agreement n° 101069690 and funded through the UKRI Horizon Europe guarantee scheme (Innovate UK project 10044059)