Multi-User Facility for SAXS/WAXS Studies on Nanoscale Structures in Controlled Environments.

Lead Research Organisation: University of Leeds
Department Name: School of Food Science and Nutrition

Abstract

It is proposed to acquire a latest-generation, state-of-the-art Small- and Wide Angle X-ray Scattering (SAXS/WAXS) instrument to versatile research capability for the characterization of nano- and mesostructure of materials and products, their application and their processing, under control of environmental conditions. Examples of research range include samples as diverse as highly ordered liquid crystals, amorphous powders, dense high performance alloys and dilute protein solutions. SAXS and WAXS provide structural information in two complementary length scale regimes, with SAXS providing the overall size, shape and structure of particles and, in the case of bulk materials, underlying internal nanostructure in the range from 1-500 nm, while WAXS offering sub-nm (molecular level) structure for components with long range molecular order in liquid, gel and solid phases.

Recent developments in laboratory SAXS/WAXS instruments have resulted in a performance step change, for many experiments closing the gap to high brilliance Synchrotron SAXS beamlines. High intensity sources (dual and triple energy solutions), scatter-less collimation and the latest detector advances have thus opened the door to new opportunities. The facility will allow us to develop, integrate and test novel, versatile sample environments investigating material nanostructures under process and synthesis conditions.

The instrument will operate as a multi-user and multidisciplinary SAXS/WAXS research facility at Harwell, under the University of Leeds (UoL) strategic relationship with the Diamond Light Source. It will (i) be a rich scientific access point of excellence for UoL and UK stakeholders who are expected to share more than 160 days of experimental beamtime per year, (ii) allow the development and testing of new sample environments, (iii) act as a focus for training the next generation of X-ray scattering experts, (iv) create a facility for industry-led research, and (v) provide the nucleus for a Network of Excellence Initiative that will strengthen and connect activities to other local SAXS-Labs in the UK.

In addition to a large core team of experienced staff, a highly qualified technician will support the maintenance of the instrument, and most importantly, support all internal and external users who access this SAXS/WAXS equipment. We also request travel funds to cover the expenses of the UoL and DLS partners travelling between institutions.

Such a capability opens up new horizons for the characterisation of complex soft matter, polymers, metals and alloys, bio-materials and advanced solid materials used in sectors such as pharmacy and healthcare, food, fine chemicals, information and communications technology (ICT), energy, process engineering and manufacturing.

Planned Impact

In terms of economic impact, both the University of Leeds and Diamond Light Source have a long- standing track record in in applied research by collaboration with industrial users, by providing commercial measurement service, as well as by spin-out and creation of IP licences. The Multi-User Facility for Small- and Wide Angle X-ray Scattering (MUseSWAXS) sited at the Harwell campus will benefit from UoL's high integration with the Industrial Liaison Office at Diamond, providing an established and well-advertised route for proprietary industrial access covering 15 different research areas, including Food, Consumer Products, Electronics, Energy, Fuels, Engineering and Healthcare to mention the most relevant areas. Industrial users will further benefit from the integrated Development Lab for designing new experimental methods (combining for instance ultrasound with X-ray scattering) and for developing novel sample-manipulation stages.

In terms of people, access to the multi-user facility and working with the top-class SAXS/WAXS equipment will enhance the professional skills of post doctorial researches and that of PhD students. Our close bonds with 8 EPSRC Centres for Doctorial Training (CDT), for instance with Soft Matter and Functional Interfaces (SOFI) and for Complex Particulate Products and Processes (cP3) will ensure that early career training will underpin collaboration with the wide range of industrial partners supporting our CDT studentships. Additionally, throughout the regularly held workshops, industrial collaborators and students national-wide will benefit as part of our research-led teaching programme.

In terms of knowledge, the expected top-class research results will affect other academic researchers internationally through their dissemination via publication in high-impact journals and at national and international conferences. Further, the cross-discipline applicants are active members of various national and international networks that will enhance dissemination even further and provide networking with world-leading scholars of materials science and engineering.

In terms of wider societal benefits, the new facility will impact on a wide range of consumer sectors, which are reflected well with the EPSRC themes Physical Sciences, Energy, Engineering, Healthcare Technologies and Manufacturing the Future. Finally, we will ensure to communicate all established societal and economic benefits enabled by the MUseSWAXS to policy makers, the wider public, charities and other research funders.

Publications

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Spooner E (2023) Air-Knife-Assisted Spray Coating of Organic Solar Cells in ACS Applied Materials & Interfaces

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Huang R (2022) Charge screening wormlike micelles affects extensional relaxation time and noodle formation. in Chemical communications (Cambridge, England)

 
Description Nine papers of users have been published in 2022 (see publication list). The type of publications concerns a wide range of materials research, with applications in energy (solid state battery research), in medicine (HSV-1infections and various cancer cell studies), in polymer design (novel elastomers) and food (milk fat research). The quality of the publications is excellent, as the list of high impact journals demonstrate. In particular order the users published in JACS, Angewandte Chemie, Macromolecules, Chemical Communications, Molecular Pharmaceutics, ACS Matereials& Interfaces, Crystal Growth & Design, Nanomaterials as well as Nanoscale.
Exploitation Route Also in the past year until mid March 2023 the DL SAXS Facility at the Diamond Light Sources was open to users. From January 2022 to mid March 2023 was fully booked, in which 50% of the instrument was used for proposed SAXS/WAXS experiments applied to the field of (bio)-materials research, 25% was reserved for activities of the experimental development lab, 10% for training /workshops and 15% for maintenance of the instrument.

I note, that every user group received training on the instrument to the beginning of their experimental session. All user groups have been successfully trained on the use of the instrument and also on the use of data reduction software DAWN.
Sectors Agriculture, Food and Drink,Chemicals,Energy,Healthcare,Manufacturing, including Industrial Biotechology,Pharmaceuticals and Medical Biotechnology

URL https://www.diamond.ac.uk/Instruments/Soft-Condensed-Matter/small-angle/Offline-SAXS.html
 
Description As demonstrated by the publications of 2022, several studies have contributed to the applied research in the fields of energy, pharmacy & medicine and food. In particular, work has been dedicated to optimising solid-state composite batteries, to drug delivery in cancer cell cures (CD-44 positive cells as well as colorectal cancer cells), to the design of gels against infections (HSV-1 infection) as well as to the optimisation of milk fat composition for the design of butter adapted for hot climates.
First Year Of Impact 2022
Sector Agriculture, Food and Drink,Energy,Pharmaceuticals and Medical Biotechnology
 
Description Diamond-Leeds Partnership Overview 
Organisation Diamond Light Source
Department Beam Instrumentation
Country United Kingdom 
Sector Private 
PI Contribution At the University of Leeds there are six partners contributing to this project; namely, (i) the School of Food Science & Nutrition, (ii) the School of Physics & Astronomy, (iii) the School of Chemistry, (iv) the School of Chemical & Process Engineering, (v) the School of Mechanical Engineering and (vi) the Faculty of Biological Sciences (FBS). The management team (Michael Rappolt, Sven Schroeder from Leeds and Nick Terrill from Diamond) are in close contact with the partners and communicate important news to the newly installed contact points. Each partner does have now a so-called 'Diamond-Leeds SAXS Facility Champion', which keep close contact with the management team of the DL-SAXS Facility and help to distribute important news at their Schools, such as, the first open call for Mailing-In Experiments in February 2021. The collaboration of the University of Leeds with the Diamond Light Source Ltd. is regulated by the Diamond-Leeds Collaboration Agreement, which has been signed in April 2019.
Collaborator Contribution The University match funding of this project (20%) has been split into two parts. That is, 75% were covered by the University of Leeds (central funding) and 25% are covered by the six University partners mentioned above. Their contribution consisted in a one payoff of about £10k and a yearly contribution of about £1.7k for the technician's salary. Note, the technician Sam Burholt was employed at the School of Food Science & Nutrition in May 2019. However, his work place is at Diamond at the DL-SAXS Facility. The collaboration partner of the University of Leeds is the Diamond Light Source Ltd (DLS). Investments from DLS for lab-refurbishment and general estates costs are estimated with about £300k. Further, DLS contributes to the project with 3.75 hours per week from Nick Terrill's working time, who is part of the DL-SAXS Facility management team.
Impact After the installation of the Xenocs SAXS-instrument at the Diamond site (Summer 2019), the foreseen commissioning period at the DL-SAXS Facility took longer than expected. Only in August 2020 did the management team agree to give approval to the delivered instrument. This longer than foreseen commissioning period was caused by two factors mainly. First, it must be noted that the instrument just does not come as one part (it is not a 'ready from the shelf' product), but contains various components from different suppliers (e.g., X-ray light source from Excillum and special detectors from Dectris AG) as well as contains a bespoke sample environment that is not standard. Making all these components work flawlessly for the first time, was expected to be not trivial. Nevertheless, the second an more influential reason for delay concerns COVID-19, which slowed down considerably all necessary technical work-tasks and necessary testing of the instrument. Nonetheless, with beginning of 2021 the DL-SAXS Facility is now fully operational and a first open call for Mailing-In Experiments has been launched in February 2021. Hereby, we are using Diamond's user access system, which has been made available for Leeds users through a Rapid Access route. Scientific outcomes in the fields of physics, chemistry, biology and engineering are expected to be reported next year.
Start Year 2018